A method for preparing a material chip

Abstract

The present invention provides a method for preparing a material chip, comprising a deposition step, a curing step, a developing step, and a baking step; each precursor solution prepares a target film at different parts of a substrate according to the deposition step, the curing step, the developing step, and the baking step, and finally performs an annealing treatment uniformly to obtain a discrete material chip; or each precursor solution forms a target film on a substrate according to the deposition step, and then the substrate with the target film is baked, and the deposition step and the baking step are cyclically performed to prepare a stacked target film at the same part of the substrate, and finally performs an annealing treatment uniformly to obtain a continuous film chip. The present invention first performs deposition to obtain a target film, and then places a mask plate, and after curing, adds a developer to obtain a target chip, effectively reducing costs, and solving the problem in the prior art that the size of the actual deposited film is smaller than the size of the mask plate due to the obstruction of the edge of the mask plate.

Description

Technical Field

[0001] The present invention relates to the field of material chips, and in particular to a method for preparing a material chip. Background Art

[0002] In the current research and development of new materials, the vast majority of new materials are developed based on the "trial and error method" of the "hypothesis-experimental verification-change parameters-experimental verification" process. This method has played an important role in the discovery of new materials. However, due to the lack of systematicity of this method and the inability to ensure consistent experimental conditions, the experiment cannot be repeated, or the change of small experimental parameters causes a large deviation in the experimental results, which leads to a long time for the development of new materials. The development of new materials based on the "trial and error method" requires a long time to complete the entire process from research and development to application, and the long research and development cycle has become an urgent problem to be solved in the development of new materials. As a new idea and new technology that has emerged in recent years, material genetic engineering aims to accelerate the development of new materials. Material genetic engineering transforms the traditional material development based on the "trial and error method" into a relationship modeling based on big data and artificial intelligence to accelerate the process of new material development. In material genes, the acquisition of big data is a key link in accelerating material research and development, and in order to obtain big data of related materials, high-throughput preparation of materials is an important means to obtain big data.

[0003] The so-called high-throughput preparation is to first combine the materials of different components in a specific order and proportion. When combining, different mask plates can be selected according to different screening purposes, such as continuous or discrete mask plates; or different mask patterns can be used, such as round or square. Then the prepared thin films of different components are homogenized and annealed to ensure that they form a uniform phase structure; finally, through a batch preparation, a high-throughput thin film chip with different components is prepared on a substrate for performance screening. The preparation of high-throughput thin film chips places strict requirements on the material preparation method. The traditional preparation method of thin film materials is mainly used for the preparation of single-component samples, which is difficult to meet the requirements of high-throughput preparation. Based on this, high-throughput preparation equipment came into being.

[0004] At present, the high-throughput preparation technology of thin films is mainly based on the existing thin film preparation system, combined with the mask system. Such as pulse laser high-throughput preparation system, magnetron sputtering high-throughput preparation system, thermal evaporation high-throughput preparation system and chemical vapor deposition high-throughput preparation system. On the one hand, when these devices are used for the preparation of high-throughput thin film materials, they need to be carried out in a vacuum environment, and the required vacuum degree varies depending on the prepared materials. However, a two-stage vacuum system, that is, a mechanical pump + a molecular pump, is generally required. In these preparation equipment, the acquisition of the vacuum environment requires large-scale cavity equipment, combined with the corresponding vacuum pump, vacuum measurement system, etc., which leads to the high price of the relevant preparation equipment. At the same time, the corresponding equipment is large in size and difficult to promote and use on a large scale. On the other hand, when the mask system used in these systems prepares discrete component points, the size of the actual deposited film is smaller than the size of the mask due to the obstruction of the edge of the mask. In particular, when the aperture of the mask is small, the effect is more obvious. Summary of the invention

[0005] The main technical problem solved by the present invention is that the prior art adopts a high-cost vacuum system when preparing material chips, resulting in high process costs, and is unable to prepare multiple discrete component points at the same time, and the operation is cumbersome and time-consuming.

[0006] According to the first aspect, an embodiment provides a method for preparing a material chip, comprising:

[0007] Different precursor solutions are prepared according to the requirements of the material chip, and each precursor solution is used to prepare a discrete material chip and / or a continuous thin film chip according to the following steps;

[0008] A deposition step, comprising depositing a precursor solution on a substrate to form a target film;

[0009] A curing step, comprising placing a mask on a substrate having the target film and performing a curing process;

[0010] A developing step, comprising adding a developing solution after the curing treatment to perform a developing treatment, and after the treatment is completed, removing the mask from the substrate having the target film;

[0011] A baking step, comprising baking the substrate having the target film after the development process;

[0012] Each precursor solution is respectively subjected to the deposition step, the curing step, the developing step and the baking step to prepare a target thin film at different positions of the substrate, and finally uniformly annealed to obtain the discrete material chip;

[0013] Alternatively, each precursor solution is formed into a target film on a substrate according to the deposition step, and then the substrate with the target film is baked, and the deposition step and the baking step are repeated to prepare a stacked target film at the same position of the substrate, that is, the target film formed by the latter precursor solution is stacked on the target film formed by the former precursor solution until the total thickness of the stacked films reaches the desired thickness, and finally annealing treatment is uniformly performed to obtain the continuous film chip.

[0014] In the embodiment of the present invention, deposition is first performed to obtain a target film, and then a mask is placed. After solidification, a developer is added to obtain a target chip, which effectively solves the problem in the prior art that the size of the actual deposited film is smaller than the size of the mask due to obstruction of the edge of the mask.

[0015] Furthermore, if multiple discrete masks are used, high-throughput preparation of discrete material chips can be achieved, thereby improving preparation efficiency. This preparation method has the advantages of being fast, low-cost, and high-throughput.

[0016] In some embodiments, the depositing is liquid phase deposition.

[0017] In some embodiments, during deposition, the precursor solution is dripped onto the substrate and then rotated so that the precursor solution forms a uniform thin film on the substrate. This step can be performed using existing glue dripping equipment.

[0018] In some embodiments, the rotation conditions are selected from at least one of the following conditions:

[0019] A1) The speed is 500-1000 rpm and the time is 5-15 seconds, which is low-speed rotation;

[0020] A2) The speed is 2000-4000 rpm and the time is 10-90 seconds, which is high-speed rotation.

[0021] In some embodiments, when rotating at a low speed, the rotation speed includes but is not limited to 500 rpm, 550 rpm, 600 rpm, 650 rpm, 700 rpm, 750 rpm, 800 rpm, 850 rpm, 900 rpm, 950 rpm, and 1000 rpm.

[0022] In some embodiments, when rotating at a low speed, the time includes but is not limited to 5 seconds, 6 seconds, 7 seconds, 8 seconds, 9 seconds, 10 seconds, 11 seconds, 12 seconds, 13 seconds, 14 seconds, 15 seconds, etc.

[0023] In some embodiments, during high-speed rotation, the rotation speed includes but is not limited to 2000 rpm, 2500 rpm, 3000 rpm, 3500 rpm, 4000 rpm, etc.

[0024] In some embodiments, when rotating at a high speed, the time includes but is not limited to 10 seconds, 20 seconds, 30 seconds, 40 seconds, 50 seconds, 60 seconds, 70 seconds, 80 seconds, 90 seconds, etc.

[0025] In some embodiments, the substrate is selected from at least one of quartz glass and silicon wafer.

[0026] In some embodiments, the curing method is laser curing or ultraviolet light curing.

[0027] In a preferred embodiment, the wavelength of the laser or ultraviolet light is 200-600 nm.

[0028] In some embodiments, if laser curing is used, the curing time is 0.5-30 minutes.

[0029] In some embodiments, the laser curing time includes but is not limited to 0.5 min, 0.6 min, 0.7 min, 0.8 min, 0.9 min, 1 min, 2 min, 3 min, 4 min, 5 min, 6 min, 7 min, 8 min, 9 min, 10 min, 11 min, 12 min, 13 min, 14 min, 15 min, 16 min, 17 min, 18 min, 19 min, 20 min, 21 min, 22 min, 23 min, 24 min, 25 min, 26 min, 27 min, 28 min, 29 min, 30 min and the like.

[0030] In some embodiments, if ultraviolet light curing is adopted, the curing time is 3 to 60 minutes.

[0031] In some embodiments, the UV curing time includes but is not limited to 3 min, 4 min, 5 min, 6 min, 7 min, 8 min, 9 min, 10 min, 11 min, 12 min, 13 min, 14 min, 15 min, 16 min, 17 min, 18 min, 19 min, 20 min, 21 min, 22 min, 23 min, 24 min, 25 min, 26 min, 27 min, 28 min, 29 min, 30 min, 35 min, 40 min, 45 min, 50 min, 55 min, 60 min and the like.

[0032] In some embodiments, the mask thickness is 0.1-0.5 mm. In some embodiments, the mask thickness includes but is not limited to 0.1 mm, 0.2 mm, 0.3 mm, 0.4 mm, 0.5 mm, etc.

[0033] In some embodiments, the mask is selected from at least one of a discrete mask and a continuous mask.

[0034] In some embodiments, when the mask is a discrete mask, the graphic size of the discrete mask is selected from at least one of the following graphic sizes:

[0035] B1) round, with a diameter of 0.1 to 1 mm;

[0036] B2) Square, side length 0.1-1 mm;

[0037] B3) Equilateral triangle, side length is 0.1~1mm.

[0038] In some embodiments, the diameter of the circular mask includes but is not limited to 0.1 mm, 0.2 mm, 0.3 mm, 0.4 mm, 0.5 mm, 0.6 mm, 0.7 mm, 0.8 mm, 0.9 mm, 1 mm, etc.

[0039] In some embodiments, the side length of the square mask includes but is not limited to 0.1 mm, 0.2 mm, 0.3 mm, 0.4 mm, 0.5 mm, 0.6 mm, 0.7 mm, 0.8 mm, 0.9 mm, 1 mm, etc.

[0040] In some embodiments, the side length of the equilateral triangle mask includes but is not limited to 0.1 mm, 0.2 mm, 0.3 mm, 0.4 mm, 0.5 mm, 0.6 mm, 0.7 mm, 0.8 mm, 0.9 mm, 1 mm, etc.

[0041] In some embodiments, when the mask is a continuous mask, the graphic size of the continuous mask is selected from at least one of the following graphic sizes:

[0042] C1) round, with a diameter of 4 to 100 mm;

[0043] C2) Square, side length 10-50 mm;

[0044] C3) Equilateral triangle: side length is 10 to 50 mm.

[0045] In some embodiments, the diameter of the circular mask includes but is not limited to 4 mm, 5 mm, 8 mm, 10 mm, 20 mm, 30 mm, 40 mm, 50 mm, 60 mm, 70 mm, 80 mm, 90 mm, 100 mm, and the like.

[0046] In some embodiments, the side length of the square mask includes but is not limited to 10 mm, 15 mm, 20 mm, 25 mm, 30 mm, 35 mm, 40 mm, 45 mm, 50 mm, etc.

[0047] In some embodiments, the side length of the equilateral triangle mask includes but is not limited to 10 mm, 15 mm, 20 mm, 25 mm, 30 mm, 35 mm, 40 mm, 45 mm, 50 mm, etc.

[0048] In some embodiments, the developer is selected from methanol, ethanol, or a combination of both.

[0049] In some embodiments, the developing time is 10 s to 70 min.

[0050] In some embodiments, the raw material of the precursor solution is selected from at least one of barium acetate, strontium acetate, tetrabutyl titanate, ethylene glycol methyl ether, acetylacetone, lead acetate, methanol, ethanol, glacial acetic acid, and ruthenium chloride. The above raw materials are only a partial list, and other raw materials may also be used.

[0051] In some embodiments, the solvent of the precursor solution is selected from at least one of formic acid, aqueous acetic acid, ethylene glycol methyl ether, and glacial acetic acid.

[0052] In some embodiments, the precursor solution is selected from at least one of strontium titanate solution, barium titanate solution, lead titanate solution, barium-doped strontium titanate solution, strontium-doped barium titanate solution, ruthenium-doped barium titanate solution, ruthenium-doped strontium titanate solution, barium titanate, and strontium ruthenate. The above solutions are only partial examples, and other solutions may also be used.

[0053] In some embodiments, the concentration of the precursor solution is 0.05-4mol / L, or 0.05-3mol / L, or 0.1-4mol / L, or 0.1-3.5mol / L, or 0.15-3.5mol / L, or 0.15-3mol / L, or 0.2-3mol / L, or 0.3-3mol / L, or 0.5-3mol / L, or 0.8-3mol / L, or 1-3mol / L, or 2-3mol / L, or 1-4mol / L, or 2-4mol / L.

[0054] In some embodiments, the concentration of the precursor solution includes but is not limited to 0.05mol / L, 0.1mol / L, 0.15mol / L, 0.2mol / L, 0.25mol / L, 0.3mol / L, 0.35mol / L, 0.4mol / L, 0.45mol / L, 0.5mol / L, 0.55mol / L, 0.6mol / L, 0.65mol / L, 0.7mol / L, 0.75mol / L, 0.8mol / L, 0.85mol / L, 0.9mol / L, 0.95mol / L, 1mol / L, 1.5mol / L, 2mol / L, 2.5mol / L, 3mol / L, 3.5mol / L, and 4mol / L.

[0055] In some embodiments, during baking, the temperature is 100-500° C. and the time is 1-5 min.

[0056] In some embodiments, the annealing temperature is 500-800° C., and the annealing time is 30-500 min.

[0057] In some embodiments, the annealing temperature includes, but is not limited to, 500°C, 550°C, 600°C, 650°C, 700°C, 750°C, 800°C.

[0058] In some embodiments, the annealing time includes but is not limited to 30 min, 40 min, 50 min, 60 min, 70 min, 80 min, 90 min, 100 min, 150 min, 200 min, 250 min, 300 min, 350 min, 400 min, 450 min, 500 min, and the like.

[0059] In some embodiments, the material chip includes but is not limited to a piezoelectric film chip, a pyroelectric film chip, a dielectric film chip, a thermoelectric film chip, and a photoelectric film chip.

[0060] In some embodiments, the substrate can be in various desired shapes, including but not limited to triangle, square, circle, hexagon, octagon, etc.

[0061] According to the second aspect, an embodiment provides a material chip made by the above method.

[0062] In some embodiments, the material chip includes but is not limited to a piezoelectric film chip, a pyroelectric film chip, a dielectric film chip, a thermoelectric film chip, and a photoelectric film chip.

[0063] In one embodiment of the present invention, deposition is first performed to obtain a target film, and then a mask is placed. After solidification, a developer is added to obtain a target chip, which effectively solves the problem in the prior art that the size of the actual deposited film is smaller than the size of the mask due to obstruction of the edge of the mask, and no longer uses a vacuum system, effectively reducing process costs.

[0064] In one embodiment of the present invention, if a plurality of discrete masks are used, high-throughput preparation of discrete material chips can be achieved, thereby improving preparation efficiency. BRIEF DESCRIPTION OF THE DRAWINGS

[0065] Figure 1 Shown is a schematic diagram of the preparation principle of a discrete thin film chip according to an embodiment of the present invention;

[0066] Figure 2 It is a schematic diagram of a discrete thin film chip according to Embodiment 1 of the present invention;

[0067] Figure 3 Shown is a schematic diagram of a continuous thin film chip according to Example 2 of the present invention.

[0068] Figure 4 Shown is a discrete thin film chip image of Comparative Example 1.

[0069] Figure 5 A material chip image showing that the actual component point side length is smaller than the mask side length.

[0070] Figure 6 It shows a material chip diagram in which the side length of the component point is consistent with the side length of the mask plate in an embodiment of the present invention. DETAILED DESCRIPTION

[0071] The present invention is further described in detail below by specific embodiments in conjunction with the accompanying drawings. Wherein similar elements in different embodiments adopt associated similar element numbers. In the following embodiments, many detailed descriptions are for making the present application better understood. However, those skilled in the art can easily recognize that some features can be omitted in different situations, or can be replaced by other elements, materials, methods. In some cases, some operations related to the present application are not shown or described in the specification, this is to avoid the core part of the present application being overwhelmed by too much description, and for those skilled in the art, it is not necessary to describe these related operations in detail, and they can fully understand the related operations according to the description in the specification and the general technical knowledge in the art.

[0072] In addition, the features, operations or characteristics described in the specification can be combined in any appropriate manner to form various implementations. At the same time, the steps or actions in the method description can also be interchanged or adjusted in a manner that is obvious to those skilled in the art. Therefore, the various sequences in the specification and the drawings are only for the purpose of clearly describing a certain embodiment and are not meant to be a required sequence, unless otherwise specified that a certain sequence must be followed.

[0073] In some embodiments, the present invention aims to provide a method for preparing a material chip, the preparation principle of which is as follows: Figure 1 As shown. It mainly includes the following steps: (1) preparing a precursor solution and designing a corresponding mask; (2) using a chemical solution deposition method to prepare a target film on a substrate; (3) using a mask combined with curing and developing technology to prepare discrete component points; (4) using solutions of different concentrations and different components to repeat the above process to achieve multi-components; (5) annealing the prepared film to make it uniform, so as to prepare a high-throughput film with different components. The method disclosed in the present invention uses a chemical solution method combined with a mask, curing, etc. to achieve high-throughput preparation of material chips, and has the advantages of simple equipment requirements, convenient operation, and conducive to industrialization.

[0074] In some embodiments, the method of the present invention does not require the use of vacuum and can be operated in an atmospheric environment, and the equipment requirements are simple. In addition, the traditional method cannot prepare multiple discrete component points, while the present invention can prepare multiple discrete component points at the same time, and can use solutions of different components and concentrations to achieve high-throughput preparation, which is easy to promote on a large scale. The present invention uses photomask technology to ensure that the component points are basically consistent with the size of the mask when preparing small-sized component points. In some embodiments, the present invention can also be used to prepare continuous thin film chips.

[0075] In some embodiments, the present invention can be used to prepare various types of functional materials, including but not limited to piezoelectric thin film chips, pyroelectric thin film chips, dielectric thin film chips, thermoelectric thin film chips, optoelectronic thin film chips, and the like.

[0076] In a first aspect, in some embodiments, the present invention provides a method for preparing a material chip, comprising:

[0077] Different precursor solutions are prepared according to the requirements of the material chip, and each precursor solution is used to prepare a discrete material chip and / or a continuous thin film chip according to the following steps;

[0078] A deposition step, comprising depositing a precursor solution on a substrate to form a target film;

[0079] A curing step, comprising placing a mask on a substrate having the target film and performing a curing process;

[0080] A developing step, comprising adding a developing solution after the curing treatment to perform a developing treatment, and after the treatment is completed, removing the mask from the substrate having the target film;

[0081] A baking step, comprising baking the substrate having the target film after the development process;

[0082] Each precursor solution is respectively subjected to the deposition step, the curing step, the developing step and the baking step to prepare a target thin film at different positions of the substrate, and finally uniformly annealed to obtain the discrete material chip;

[0083] Alternatively, each precursor solution is formed into a target film on a substrate according to the deposition step, and then the substrate with the target film is baked, and the deposition step and the baking step are repeated to prepare a stacked target film at the same position of the substrate, that is, the target film formed by the latter precursor solution is stacked on the target film formed by the former precursor solution until the total thickness of the stacked films reaches the desired thickness, and finally annealing treatment is uniformly performed to obtain the continuous film chip.

[0084] The present invention combines the curing step with the developing step to successfully prepare discrete component dots.

[0085] Herein, a discrete material chip refers to a material chip having multiple discrete points.

[0086] Herein, a continuous material chip refers to a material chip with at least one thin film spin-coated thereon. The continuous material chip can be made by spin-coating solutions of different concentrations on the same area of ​​a substrate, or by spin-coating solutions of different concentrations on different areas.

[0087] Herein, the precursor solution refers to the solution used to deposit the thin film.

[0088] Herein, the mask plate may also be referred to as a mask plate, a mask plate or a mask.

[0089] In some embodiments, the precursor solution can be prepared in advance and allowed to stand for 24-120 hours before use. The standing time includes but is not limited to 24 hours, 48 ​​hours, 72 hours, 96 hours, 120 hours, and the like.

[0090] In some embodiments, the raw material of the precursor solution is selected from at least one of barium acetate, strontium acetate, tetrabutyl titanate, ethylene glycol methyl ether, acetylacetone, lead acetate, methanol, ethanol, glacial acetic acid, and ruthenium chloride. The above raw materials are only a partial list, and other raw materials may also be used.

[0091] In some embodiments, the solvent of the precursor solution is selected from at least one of formic acid, aqueous acetic acid, ethylene glycol methyl ether, and glacial acetic acid. The aqueous acetic acid may be an acetic acid aqueous solution with a mass fraction of 36%, and the glacial acetic acid refers to anhydrous acetic acid.

[0092] In some embodiments, the precursor solution is selected from at least one of strontium titanate solution, barium titanate solution, lead titanate solution, barium-doped strontium titanate solution, strontium-doped barium titanate solution, ruthenium-doped barium titanate solution, ruthenium-doped strontium titanate solution, barium titanate, and strontium ruthenate. The solvent of the above solution can generally contain two or more solvents, for example, it can be a mixed solvent composed of glacial acetic acid and ethylene glycol methyl ether. The above solution is only a partial list, and other solutions can also be used.

[0093] In some embodiments, the precursor solution further contains a stabilizer, which includes but is not limited to acetylacetone and the like.

[0094] In some embodiments, the concentration of the precursor solution is 0.05-4mol / L, or 0.05-3mol / L, or 0.1-4mol / L, or 0.1-3.5mol / L, or 0.15-3.5mol / L, or 0.15-3mol / L, or 0.2-3mol / L, or 0.3-3mol / L, or 0.5-3mol / L, or 0.8-3mol / L, or 1-3mol / L, or 2-3mol / L, or 1-4mol / L, or 2-4mol / L.

[0095] In some embodiments, the concentration of the precursor solution includes but is not limited to 0.05mol / L, 0.1mol / L, 0.15mol / L, 0.2mol / L, 0.25mol / L, 0.3mol / L, 0.35mol / L, 0.4mol / L, 0.45mol / L, 0.5mol / L, 0.55mol / L, 0.6mol / L, 0.65mol / L, 0.7mol / L, 0.75mol / L, 0.8mol / L, 0.85mol / L, 0.9mol / L, 0.95mol / L, 1mol / L, 1.5mol / L, 2mol / L, 2.5mol / L, 3mol / L, 3.5mol / L, 4mol / L and the like.

[0096] In some embodiments, the depositing is liquid phase deposition.

[0097] In some embodiments, during deposition, the precursor solution is dripped onto the substrate and then rotated so that the precursor solution forms a uniform thin film on the substrate. Existing glue dripping equipment can be used for glue dripping.

[0098] In some embodiments, the rotation conditions are selected from at least one of the following conditions:

[0099] A1) The speed is 500-1000 rpm and the time is 5-15 seconds, which is low-speed rotation;

[0100] A2) The rotation speed is 2000-4000 rpm and the time is 10-90 seconds, which is high-speed rotation.

[0101] In some embodiments, when rotating at a low speed, the rotation speed includes but is not limited to 500 rpm, 550 rpm, 600 rpm, 650 rpm, 700 rpm, 750 rpm, 800 rpm, 850 rpm, 900 rpm, 950 rpm, and 1000 rpm.

[0102] In some embodiments, when rotating at a low speed, the time includes but is not limited to 5 seconds, 6 seconds, 7 seconds, 8 seconds, 9 seconds, 10 seconds, 11 seconds, 12 seconds, 13 seconds, 14 seconds, 15 seconds, etc.

[0103] In some embodiments, during high-speed rotation, the rotation speed includes but is not limited to 2000 rpm, 2500 rpm, 3000 rpm, 3500 rpm, 4000 rpm, etc.

[0104] In some embodiments, when rotating at a high speed, the time includes but is not limited to 10 seconds, 20 seconds, 30 seconds, 40 seconds, 50 seconds, 60 seconds, 70 seconds, 80 seconds, 90 seconds, etc.

[0105] In some embodiments, the low speed rotation described in A1) is performed first, and then the high speed rotation described in A2) is performed.

[0106] In some embodiments, the substrate is selected from at least one of quartz glass and silicon wafer.

[0107] In some embodiments, the curing method is laser curing or ultraviolet light curing.

[0108] Preferably, the wavelength of the laser or ultraviolet light is 200-600 nm, including but not limited to 200 nm, 250 nm, 300 nm, 350 nm, 400 nm, 450 nm, 500 nm, 550 nm, and 600 nm.

[0109] In some embodiments, if laser curing is used, the curing time is 0.5 to 30 minutes, including but not limited to 0.5 minutes, 0.6 minutes, 0.7 minutes, 0.8 minutes, 0.9 minutes, 1 minute, 2 minutes, 3 minutes, 4 minutes, 5 minutes, 6 minutes, 7 minutes, 8 minutes, 9 minutes, 10 minutes, 11 minutes, 12 minutes, 13 minutes, 14 minutes, 15 minutes, 16 minutes, 17 minutes, 18 minutes, 19 minutes, 20 minutes, 21 minutes, 22 minutes, 23 minutes, 24 minutes, 25 minutes, 26 minutes, 27 minutes, 28 minutes, 29 minutes, 30 minutes and the like.

[0110] In some embodiments, if ultraviolet light curing is used, the curing time is 3 to 60 minutes.

[0111] In some embodiments, the UV curing time includes but is not limited to 3 min, 4 min, 5 min, 6 min, 7 min, 8 min, 9 min, 10 min, 11 min, 12 min, 13 min, 14 min, 15 min, 16 min, 17 min, 18 min, 19 min, 20 min, 21 min, 22 min, 23 min, 24 min, 25 min, 26 min, 27 min, 28 min, 29 min, 30 min, 35 min, 40 min, 45 min, 50 min, 55 min, 60 min and the like.

[0112] In some embodiments, the mask thickness is 0.1-0.5 mm. In some embodiments, the mask thickness includes but is not limited to 0.1 mm, 0.2 mm, 0.3 mm, 0.4 mm, 0.5 mm, and the like.

[0113] Typically, UV curing times are longer than laser curing times.

[0114] In some embodiments, the mask is selected from at least one of a discrete mask and a continuous mask.

[0115] In some embodiments, when the mask is a discrete mask, the pattern size is selected from at least one of the following sizes:

[0116] B1) round, with a diameter of 0.1 to 1 mm;

[0117] B2) Square, side length 0.1-1 mm;

[0118] B3) Equilateral triangle, side length is 0.1~1mm.

[0119] In some embodiments, the diameter of the circular mask includes but is not limited to 0.1 mm, 0.2 mm, 0.3 mm, 0.4 mm, 0.5 mm, 0.6 mm, 0.7 mm, 0.8 mm, 0.9 mm, 1 mm, etc.

[0120] In some embodiments, the side length of the square mask includes but is not limited to 0.1 mm, 0.2 mm, 0.3 mm, 0.4 mm, 0.5 mm, 0.6 mm, 0.7 mm, 0.8 mm, 0.9 mm, 1 mm, etc.

[0121] In some preferred embodiments, the side length of the equilateral triangle mask includes but is not limited to 0.1 mm, 0.2 mm, 0.3 mm, 0.4 mm, 0.5 mm, 0.6 mm, 0.7 mm, 0.8 mm, 0.9 mm, 1 mm, etc.

[0122] In some embodiments, when the mask is a continuous mask, the graphic size of the continuous mask is selected from at least one of the following graphic sizes:

[0123] C1) round, with a diameter of 4 to 100 mm;

[0124] C2) Square, side length 10-50 mm;

[0125] C3) Equilateral triangle: side length is 10 to 50 mm.

[0126] In some embodiments, the diameter of the circular mask includes but is not limited to 4 mm, 5 mm, 8 mm, 10 mm, 20 mm, 30 mm, 40 mm, 50 mm, 60 mm, 70 mm, 80 mm, 90 mm, 100 mm, and the like.

[0127] In some embodiments, the side length of the square mask includes but is not limited to 10 mm, 15 mm, 20 mm, 25 mm, 30 mm, 35 mm, 40 mm, 45 mm, 50 mm, etc.

[0128] In some embodiments, the side length of the equilateral triangle mask includes but is not limited to 10 mm, 15 mm, 20 mm, 25 mm, 30 mm, 35 mm, 40 mm, 45 mm, 50 mm, etc.

[0129] In some embodiments, the developer is selected from methanol, ethanol, or a combination of both. Specifically, it can be any one of them, or a mixed solvent of methanol and ethanol.

[0130] In some embodiments, the developing time is ≤70 min, preferably 10s to 70 min. In some embodiments, the developing time is 10 to 1200 s. In some embodiments, the developing time includes but is not limited to 10s, 20s, 50s, 80s, 100s, 130s, 150s, 180s, 200s, 250s, 300s, 400s, 500s, 600s, 700s, 800s, 900s, 1000s, 1100s, 1200s, etc. In other embodiments, the development time is 10-800s, preferably 10-700s, more preferably 10-600s, more preferably 30-600s, more preferably 50-600s, more preferably 60-600s, more preferably 80-600s, more preferably 90-600s, more preferably 100-600s, more preferably 200-600s, more preferably 300-600s, more preferably 400-600s.

[0131] In other embodiments, the developing time is 10-70 min, preferably 15-70 min, more preferably 20-70 min, more preferably 20-65 min, more preferably 20-60 min, more preferably 25-60 min, more preferably 30-60 min. In other embodiments, the developing time includes but is not limited to 20 min, 25 min, 30 min, 35 min, 40 min, 45 min, 50 min, 55 min, 60 min, 65 min, 70 min, etc.

[0132] In some embodiments, the temperature during baking is 100-500° C. and the time is 1-5 min. During baking, the polymer decomposes.

[0133] In some preferred embodiments, the baking temperature is 100-400° C. In some embodiments, the baking temperature includes but is not limited to 100° C., 150° C., 200° C., 250° C., 300° C., 350° C., 400° C., 450° C., 500° C., and the like.

[0134] In some embodiments, the annealing temperature is 500-800° C., and the annealing time is 30-500 min.

[0135] In some embodiments, the annealing temperature includes, but is not limited to, 500°C, 550°C, 600°C, 650°C, 700°C, 750°C, 800°C, and the like.

[0136] In some embodiments, the annealing time includes but is not limited to 30 min, 40 min, 50 min, 60 min, 70 min, 80 min, 90 min, 100 min, 150 min, 200 min, 250 min, 300 min, 350 min, 400 min, 450 min, 500 min, and the like.

[0137] In some embodiments, the material chip includes but is not limited to a piezoelectric film chip, a pyroelectric film chip, a dielectric film chip, a thermoelectric film chip, and a photoelectric film chip.

[0138] In some embodiments, the substrate can be in various desired shapes, including but not limited to triangle, square, and the like.

[0139] In a second aspect, the present invention provides a material chip produced by the above method.

[0140] In some embodiments, the material chip includes but is not limited to a piezoelectric film chip, a pyroelectric film chip, a dielectric film chip, a thermoelectric film chip, and a photoelectric film chip.

[0141] In the embodiment of the present invention, deposition is first performed to obtain a target film, and then a mask is placed. After solidification, a developer is added to obtain a target chip, which effectively solves the problem in the prior art that the size of the actual deposited film is smaller than the size of the mask due to obstruction of the edge of the mask.

[0142] In the prior art, such as Figure 5 As shown, the left picture is a discrete mask design drawing, the side length of the mask is 0.5mm, and the right picture is a micrograph of the material chip. When a discrete mask with a side length of 0.5mm is used to prepare a material chip, the side length of the discrete component points formed is only about 0.3mm.

[0143] In one embodiment, if Figure 6 As shown, the left picture is a discrete mask design drawing, the side length of the mask is 0.2mm, and the right picture is a micrograph of the material chip. When a discrete mask with a side length of 0.2mm is used to prepare a material chip, the side length of the discrete component points of the prepared material chip is also 0.2mm, i.e. 200μm, which effectively solves the problem in the prior art that the size of the actual deposited film is smaller than the size of the mask due to the obstruction of the edge of the mask.

[0144] Example 1

[0145] This embodiment provides discrete material chip preparation, including the following steps:

[0146] 1) using strontium acetate, acetic acid, ethylene glycol methyl ether, tetrabutyl titanate, neodymium chloride, dysprosium acetate, and lanthanum chloride as raw materials, and using acetic acid and ethylene glycol methyl ether as solvents, preparing strontium titanate, dysprosium-doped strontium titanate, and lanthanum-doped strontium titanate solutions of different concentrations;

[0147] 2) Using chemical liquid deposition, different drop-adding sequences were selected according to the designed ratio, first using a low speed of 500 rpm for 10 seconds, then using a high speed of 2000 rpm for 1 minute, to prepare a thin film on a silicon wafer with a size of 33 mm*33 mm*1 mm;

[0148] 3) Using a discrete mask plate (304 stainless steel), the pattern shape of the discrete mask plate is square, in a sheet-like structure, with a side length of 1 mm and 400 discrete points;

[0149] 4) placing the mask on the substrate on which the film has been prepared, and then curing the prepared film for 1200 seconds using an ultraviolet lamp with a wavelength of 200-600 nm;

[0150] 5) taking out the cured film substrate, using methanol as a developer to etch the cured film, taking out the film substrate after developing for 10 seconds, and removing the mask from the film substrate; then baking the film substrate at 200° C. for 5 minutes;

[0151] 6) Using different solutions to prepare thin films in different areas of the substrate, repeating the curing and developing steps to obtain material chips with different compositions;

[0152] 7) Finally, the prepared film is subjected to diffusion annealing at a temperature of 750° C. for 60 minutes to obtain material chips with different components.

[0153] Figure 2 The figure shows a schematic diagram of a discrete material chip. Figure 2 In the figure, the white square dots are the discrete component points, and the black areas are the recessed etching areas formed after the developer is added for development.

[0154] Performance test: The performance test of high-throughput material chips is achieved by testing their conductivity one by one. Since there are many points, we listed 154 of them. The test results are shown in Table 1 below.

[0155] Table 1 Material chip resistance distribution table (unit: kΩ)

[0156]

[0157] It can be seen from the resistance distribution in Table 1 that the present embodiment successfully produced material chips with different composition points.

[0158] Using the traditional sol-gel method to prepare thin film materials, the time required to prepare one component point is as follows:

[0159] Solution preparation: 4 hours, standing: 72-120 hours, film preparation: 3 hours; annealing 4 hours; the above process needs to be repeated for each component point prepared.

[0160] The method of this embodiment is used to prepare a high-throughput material chip, and up to 400 components can be prepared at one time, and the time is as follows:

[0161] Preparation of 4-8 solutions: 10 hours; Standing: 72-120 hours; Thin film preparation: 10 hours; Annealing: 4 hours. Effectively simplify the operation steps and shorten the preparation time.

[0162] Example 2

[0163] This embodiment provides a method for preparing a continuous thin film chip, comprising the following steps:

[0164] 1) using barium acetate, ruthenium chloride, bismuth nitrate, strontium titanate, and tetrabutyl titanate as raw materials, and using glacial acetic acid and ethylene glycol methyl ether as solvents, barium titanate, bismuth titanate, and strontium ruthenate solutions of different concentrations were prepared;

[0165] 2) A triangular substrate is used as a substrate, part of which is a silicon wafer and the other part is a glass substrate. The specific shape is an equilateral triangle with a side length of 20 mm. A chemical solution deposition method is used to spin-coat a film using solutions of different concentrations at different positions of the substrate. The spin coating parameters are: low speed 500 rpm, 10 seconds; high speed 4000 rpm, 1 minute;

[0166] 3) baking the substrate with the thin film at 200°C for 1 min and at 500°C for 5 min; then spin-coating a second thin film with solutions of different concentrations and baking, and repeating the process until a predetermined thickness is reached;

[0167] 4) Finally, the prepared film is subjected to diffusion annealing at a temperature of 700°C for 30 minutes to prepare a material chip with a continuous structure of different components, such as Figure 3 As shown, a1, b1, and c1 are spin coating positions.

[0168] Example 3

[0169] This embodiment provides the preparation of a discrete material chip, comprising the following steps:

[0170] 1) using strontium acetate, ruthenium chloride, barium acetate, and tetrabutyl titanate as raw materials, using glacial acetic acid and ethylene glycol methyl ether as solvents, and using acetylacetone as a stabilizer, preparing strontium titanate, strontium ruthenate, and barium titanate solutions of different concentrations;

[0171] 2) using chemical liquid deposition method, using low speed 800 rpm, 10 seconds, high speed 3000 rpm, 30 seconds, to prepare a thin film on a quartz substrate;

[0172] 3) Using a discrete mask, the pattern shape is a square with a side length of 2 mm; the number of discrete points is greater than 100;

[0173] 4) placing the mask on the substrate on which the thin film has been prepared, and then curing the prepared thin film with a laser for 30 seconds, with a laser wavelength of 200-600nm;

[0174] 5) Take out the cured film, use methanol as a developer to etch the cured film, and take out the film substrate after developing for 10 seconds; then bake the film at 200°C for 1 minute and 400°C for 5 minutes;

[0175] 6) Using different solutions to prepare thin films in different areas of the substrate, repeating the curing and developing steps to obtain material chips with different compositions;

[0176] 7) Finally, the prepared film is subjected to diffusion annealing at a temperature of 700° C. for 45 minutes to obtain material chips with different components.

[0177] Comparative Example 1

[0178] This comparative example provides the preparation of a discrete material chip, comprising the following steps:

[0179] 1) using strontium acetate, lead acetate, zirconium isopropoxide, barium acetate, tetrabutyl titanate as raw materials, and using glacial acetic acid and ethylene glycol methyl ether as solvents to prepare strontium titanate, strontium ruthenate and barium titanate solutions of different concentrations;

[0180] 2) using chemical liquid deposition method, using low speed 800 rpm, 10 seconds, high speed 3000 rpm, 25 seconds, to prepare a thin film on a quartz substrate;

[0181] 3) Using a discrete mask, the pattern shape is a square with a side length of 1 mm; the number of discrete points is greater than 100;

[0182] 4) placing the mask on the substrate on which the film has been prepared, and then curing the prepared film for 5 seconds using a laser or ultraviolet lamp, the wavelength of the laser or ultraviolet light being 200-600 nm;

[0183] 5) Take out the cured film, use methanol as a developer to etch the cured film, take out the film substrate after developing for 1 second, remove the mask from the film substrate; then bake the film substrate at 200°C for 1 minute and at 400°C for 5 minutes.

[0184] The discrete material chips prepared are as follows Figure 4 As shown, discrete dots cannot be formed due to insufficient curing time and developing time.

[0185] The above specific examples are used to illustrate the present invention, which is only used to help understand the present invention and is not intended to limit the present invention. For those skilled in the art, according to the concept of the present invention, some simple deductions, modifications or substitutions can be made.

Claims

1. A method for preparing a material chip, characterized in that: include: Prepare different precursor solutions according to the requirements of the material chip and let them stand for 24-120 hours before use. Each precursor solution is used to prepare a discrete material chip according to the following steps; A deposition step, comprising depositing a precursor solution on a substrate to form a target film; A curing step, comprising placing a mask on a substrate having the target film and performing a curing process; A developing step, comprising adding a developing solution after the curing treatment to perform a developing treatment, and after the treatment is completed, removing the mask from the substrate having the target film; A baking step, comprising baking the substrate having the target film after the development process; Each precursor solution is respectively subjected to the deposition step, the curing step, the developing step and the baking step to prepare a target thin film at different positions of the substrate, and finally uniformly annealed to obtain the discrete material chip; Wherein, the deposition is liquid phase deposition; during deposition, the precursor solution is dripped onto the substrate and then rotated so that the precursor solution forms a uniform thin film on the substrate; the rotation condition is first low-speed rotation and then high-speed rotation; the rotation speed of the low-speed rotation is 500-1000 rpm, and the time is 5-15 seconds; the rotation speed of the high-speed rotation is 2000-4000 rpm, and the time is 10-90 seconds; The curing method is laser curing or ultraviolet light curing; the wavelength of the laser or ultraviolet light is 200-600nm; if laser curing is adopted, the curing time is 0.5-30min; if ultraviolet light curing is adopted, the curing time is 3-60min; The developer is selected from methanol, ethanol or a combination of the two; the development treatment time is 10s to 70min; During baking, the temperature is 100-500°C and the time is 1-5 minutes; the annealing temperature of the annealing treatment is 500-800°C and the annealing time is 30-500 minutes; The raw material of the precursor solution is selected from at least one of barium acetate, strontium acetate, tetrabutyl titanate, and ruthenium chloride; the solvent of the precursor solution is selected from at least one of formic acid, aqueous acetic acid, ethylene glycol methyl ether, and glacial acetic acid; the precursor solution is selected from at least one of strontium titanate solution, barium titanate solution, lead titanate solution, barium-doped strontium titanate solution, strontium-doped barium titanate solution, ruthenium-doped barium titanate solution, ruthenium-doped strontium titanate solution, and strontium ruthenate; the concentration of the precursor solution is 0.05-4 mol / L; the aqueous acetic acid is an acetic acid aqueous solution with a mass fraction of 36%; the precursor solution also contains a stabilizer, and the stabilizer is acetylacetone.

2. The preparation method according to claim 1, characterized in that The thickness of the mask plate is 0.1 to 0.5 mm; the mask plate is selected from at least one of a discrete mask plate and a continuous mask plate; When the mask is a discrete mask, the graphic size of the discrete mask is selected from at least one of the following graphic sizes: B1) round, with a diameter of 0.1 to 1 mm; B2) Square, side length 0.1-1 mm; B3) Equilateral triangle, side length 0.1-1 mm; When the mask is a continuous mask, the pattern size of the continuous mask is selected from at least one of the following pattern sizes: C1) round, with a diameter of 4 to 100 mm; C2) Square, side length 10-50 mm; C3) Equilateral triangle: side length is 10 to 50 mm.

3. The preparation method according to claim 1, characterized in that: The substrate is selected from at least one of quartz glass and silicon wafer.

4. A material chip obtained by the preparation method according to any one of claims 1 to 3, wherein the material chip comprises a piezoelectric film chip, a pyroelectric film chip, a dielectric film chip, a thermoelectric film chip, and a photoelectric film chip.

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