Preparation method of zirconium boride slurry and zirconium boride film

Abstract

The application discloses a preparation method of zirconium boride slurry and a zirconium boride film, and comprises the following steps: (1) preparing an organic solvent; (2) adding 0.5-1.5 wt% of a dispersing agent into the organic solvent; (3) weighing zirconium boride powder and boron oxide powder with a mass ratio of 1:0.01-0.05, and adding the powder into the solution prepared in the step (2), and then performing ultrasonic dispersion after fully stirring, so that the solid phase content is 5 vol%-10 vol%; (4) placing the mixed slurry prepared in the step (3) into a homogenizer with a rotating speed of 13000-14000 r / min, and stirring for 30-60 min, so that the powder can be fully and uniformly dispersed; and (5) filtering out large particles with a particle size greater than 1 mu m, and thus the zirconium boride slurry is obtained. The solid phase content of the zirconium boride slurry is reduced to 5 vol%-10 vol%, and the organic solvent is selected as a dispersion medium, so that the stability of the zirconium boride slurry is improved, and the film formation is more favorable. The zirconium boride film is prepared by adopting a photon sintering method, the use of inert gas or reducing gas atmosphere is avoided, the sintering time is shortened, the preparation cost is reduced, and the preparation efficiency is improved.

Description

TECHNICAL FIELD

[0001] The application belongs to the technical field of coating manufacturing, and relates to a preparation method of zirconium boride slurry and a zirconium boride film. BACKGROUND

[0002] Zirconium boride (ZrB2) has the characteristics of high melting point, high strength, high hardness, good electrical conductivity and thermal conductivity, good heat resistance, flame resistance, oxidation resistance, corrosion resistance and the like, so that it is widely developed and applied in high-temperature structural ceramic materials, electrode materials, film materials, composite materials, refractory materials and the like.

[0003] There are many preparation and sintering methods of zirconium boride film coating, and common forming methods include sputtering deposition technology, chemical vapor deposition technology, pulsed laser deposition technology, electron beam evaporation technology and the like. The sintering methods include normal pressure sintering and hot-pressing sintering and the like. Since the covalent bond of zirconium boride is relatively strong, the sintering process is very difficult, and the sintering process of zirconium boride needs to be carried out in an inert atmosphere or a reducing atmosphere, so that the preparation process of zirconium boride greatly increases the cost and is extremely low in efficiency. SUMMARY

[0004] The application aims at the deficiencies of the prior art, and provides a preparation method of zirconium boride slurry and a zirconium boride film.

[0005] The application aims at the deficiencies of the prior art, and provides a preparation method of zirconium boride slurry and a zirconium boride film.

[0006] (1) configuring an organic solvent: the organic solvent is any one or a mixture of multiple ones of ethanol, ethylene glycol and glycerol in any mass ratio, and ultrasonic dispersion is performed;

[0007] (2) adding 0.5-1.5wt% of a dispersant into the organic solvent, the dispersant is any one or a mixture of multiple ones of ammonium oleate, stearic acid, triolein and castor oil in any mass ratio, uniform stirring and ultrasonic dispersion are performed;

[0008] (3) weighing zirconium boride powder and boron oxide powder in a mass ratio of 1:0.01-0.05, adding the solution prepared in step (2), fully stirring and then performing ultrasonic dispersion, and the solid phase content is 5vol%-10vol%;

[0009] (4) placing the mixed slurry prepared in step (3) into a homogenizer with a rotating speed of 13000-14000r / min, and stirring for 30-60min, so that the powder can be fully and uniformly dispersed;

[0010] (5) filtering out large particles with a particle size greater than 1um to obtain the zirconium boride slurry.

[0011] Further, in the step (1), the organic solvent is a mixed solvent prepared by mixing ethanol, ethylene glycol and glycerol in a volume ratio of 3:1:1.

[0012] Further, in the step (2), the dispersant is a mixture of ammonium oleate and stearic acid in a mass ratio of 1:2.

[0013] Further, in the step (3), the average particle size of the zirconium boride powder is 100 nm.

[0014] Further, in the steps (1) and (2), the ultrasonic dispersion time is 10-15 min, and in the step (3), the ultrasonic dispersion time is 25-30 min.

[0015] The application further provides a zirconium boride film prepared from the zirconium boride slurry prepared by the above method.

[0016] Further, the preparation method of the zirconium boride film comprises the following steps:

[0017] Step 1: selecting a non-sintered dense ceramic material as a printing substrate, the sintering temperature of the ceramic substrate being 1100℃, and performing surface treatment on the substrate;

[0018] Step 2: printing a zirconium boride film sample on the substrate using the zirconium boride slurry as a raw material;

[0019] Step 3: placing the printed sample into an oven for drying, the oven temperature being set to 60-80℃, and the time being 30 min;

[0020] Step 4: performing photonic sintering on the dried sample to obtain a zirconium boride film.

[0021] Further, the printing of the zirconium boride film on the substrate specifically comprises: drawing a film model and importing it into a corresponding software, and printing the zirconium boride film on the substrate by using an inkjet printing method.

[0022] Further, the photonic sintering specifically comprises: using a strong pulsed photonic sintering test bench, adjusting the distance between the sample and the light-emitting lamp tube to 2-4 cm, setting the total energy density to 20-40 J / cm 2 , adjusting the irradiation time to 2-5 ms, and performing photonic sintering.

[0023] Further, the surface treatment of the substrate specifically comprises: cleaning the substrate in an ultrasonic instrument using acetone, methanol and deionized water for 5-10 min, and then cleaning the substrate using an isopropyl alcohol solution for 5-10 min.

[0024] Or using sodium hydroxide (NaOH) solution to clean the substrate for 10-20 min, and then clean with deionized water again;

[0025] Or clean the substrate with deionized water in ultrasonic wave for 10-20 min;

[0026] Or using UV / O 3 The cleaning agent is used to clean the substrate for 10-20 min.

[0027] Compared with the prior art, the present application has the beneficial effects that:

[0028] 1、The solid content of the zirconium boride slurry is reduced to 5vol% to 10vol%, and only an organic solvent is selected as a dispersion medium, so that the stability of the zirconium boride slurry is improved, the film forming is more favorable, and the zirconium boride slurry can be used for photon sintering.

[0029] 2、The zirconium boride film is prepared by the method of photon sintering, the use of inert gas or reducing gas atmosphere is avoided, the sintering time is greatly shortened, the preparation cost is reduced, and the preparation efficiency is improved. BRIEF DESCRIPTION OF DRAWINGS

[0030] In order to more clearly illustrate the technical solutions in the embodiments of the present application, the drawings needed to be used in the embodiment description will be briefly introduced. Obviously, the drawings in the following description are only some embodiments of the present application, and other drawings can be obtained by those skilled in the art without creative labor.

[0031] Figure 1 It is a zirconium boride film pattern printed by the embodiment of the present application.

[0032] Figure 2 It is a thickness electron microscope graph of the zirconium boride film obtained by the embodiment 10 of the present application.

[0033] Figure 3 It is a surface electron microscope graph of the zirconium boride film obtained by the embodiment 10 of the present application.

[0034] Figure 4 It is a surface electron microscope graph of the zirconium boride film obtained by the embodiment 11 of the present application.

[0035] Figure 5 It is a thickness electron microscope graph of the zirconium boride film obtained by the embodiment 12 of the present application.

[0036] Figure 6 It is a surface electron microscope graph of the zirconium boride film obtained by the embodiment 12 of the present application. DETAILED DESCRIPTION

[0037] The application will be described in detail below with reference to the drawings. The features in the following examples and embodiments can be combined with each other without conflict.

[0038] The application also provides a preparation method of the zirconium boride slurry.

[0039] (1) The organic solvent is configured: the organic solvent is any one or more of ethanol, ethylene glycol, and glycerol in any mass ratio, and is subjected to ultrasonic dispersion;

[0040] (2) 0.5-1.5wt% of a dispersant is added to the organic solvent, the dispersant is any one or more of ammonium oleate, stearic acid, triolein, and castor oil in any mass ratio, is stirred uniformly and subjected to ultrasonic dispersion;

[0041] (3) Zirconium boride powder and boron oxide powder in a mass ratio of 1:0.01-0.05 are weighed and added to the solution configured in step (2), and are subjected to ultrasonic dispersion after being stirred fully, with a solid content of 5vol%-10vol%;

[0042] (4) The mixed slurry configured in step (3) is placed under a homogenizer with a rotation speed of 13000-14000r / min and is stirred for 30-60min, so that the powder can be dispersed fully and uniformly;

[0043] (5) Large particles with a particle size greater than 1μm formed by agglomeration are filtered out, and the zirconium boride slurry is obtained.

[0044] The calculation formula of the solid content is as follows:

[0045]

[0046] Example 1,

[0047] The application also provides a preparation method of the zirconium boride slurry.

[0048] S1, ethanol and ethylene glycol in a volume ratio of 1:1 are measured and configured into a mixed solvent, and the mixed solvent is subjected to ultrasonic dispersion for 15min, so that the two solutions are mixed uniformly.

[0049] S2, 0.75wt% of a dispersant ammonium oleate is added to the mixed solvent, and is stirred uniformly and subjected to ultrasonic dispersion for 15min. The mass ratio of the mixed powder (zirconium boride powder and boron oxide powder) to the dispersant is 1:0.75, the mass of the mixed powder added is fixed, which is determined by the solid content, and the amount of the dispersant added is determined according to the mixed powder, and the dispersant is added first and then the mixed powder is added after the amount is determined.

[0050] S3, boron zirconium powder and boron oxide powder with a mass ratio of 1:0.01 are weighed and added to the solution prepared in step S2, and after sufficient stirring, ultrasonic dispersion is performed for 30 min;

[0051] S4, the mixed powder slurry prepared in step S3 is placed into an adjustable high-speed homogenizer with a rotating speed of 14000 r / min for stirring for 30 min, so that the powder can be fully and uniformly dispersed.

[0052] S5, the mixed boron zirconium slurry is filtered by using a needle type filter membrane filter (organic) with a pore size of 1 μm to remove large particles formed by agglomeration in the slurry.

[0053] Example 2,

[0054] A preparation method of a boron zirconium slurry, comprising the following steps:

[0055] S1, ethanol and ethylene glycol with a volume ratio of 1:1 are weighed to prepare a mixed solvent, and the mixed solvent is ultrasonically dispersed for 15 min to uniformly mix the two solutions.

[0056] S2, 0.75wt% of a dispersant stearic acid is added to the mixed solvent, stirred uniformly and ultrasonically dispersed for 15 min. The mass ratio of the mixed powder (boron zirconium powder and boron oxide powder) to the dispersant is 1:0.75, the mass of the mixed powder added is fixed, which is determined by the solid content, and the amount of the dispersant added is determined according to the mixed powder. After determining the amount, the dispersant is added first and then the mixed powder is added.

[0057] S3, boron zirconium powder and boron oxide powder with a mass ratio of 1:0.01 are weighed and added to the solution prepared in step S2, and after sufficient stirring, ultrasonic dispersion is performed for 30 min;

[0058] S4, the mixed powder slurry prepared in step S3 is placed into an adjustable high-speed homogenizer with a rotating speed of 14000 r / min for stirring for 30 min, so that the powder can be fully and uniformly dispersed.

[0059] S5, the mixed boron zirconium slurry is filtered by using a needle type filter membrane filter (organic) with a pore size of 1 μm to remove large particles formed by agglomeration in the slurry.

[0060] Example 3,

[0061] A preparation method of a boron zirconium slurry, comprising the following steps:

[0062] S1, ethanol and ethylene glycol with a volume ratio of 1:1 are weighed to prepare a mixed solvent, and the mixed solvent is ultrasonically dispersed for 15 min to uniformly mix the two solutions.

[0063] S2, 0.75wt% dispersant glyceryl trioleate is added to the mixed solvent, stirred uniformly and ultrasonic dispersed for 15 min. Among them, the mass ratio of mixed powder (zirconium boride powder and boron oxide powder) to dispersant is 1:0.75, the mass of mixed powder added is fixed, which is determined by solid content, and the amount of dispersant added is determined according to the mixed powder. After determining the amount, add the dispersant first and then add the mixed powder.

[0064] S3, zirconium boride powder and boron oxide powder with a mass ratio of 1:0.03 are weighed and added to the solution prepared in step S2, and then fully stirred and ultrasonic dispersed for 30 min;

[0065] S4, the mixed powder slurry prepared in step S3 is placed in a adjustable high-speed homogenizer with a rotating speed of 14000r / min and stirred for 30 min, so that the powder can be fully and uniformly dispersed.

[0066] S5, the mixed zirconium boride slurry is filtered by a needle type filter membrane filter (organic) with a pore size of 1μm to remove large particles formed by agglomeration in the slurry.

[0067] Example 4,

[0068] A preparation method of zirconium boride slurry, comprising the following steps:

[0069] S1, ethanol and ethylene glycol with a volume ratio of 1:1 are prepared into a mixed solvent, and the mixed solvent is ultrasonic dispersed for 15 min to uniformly mix the two solutions.

[0070] S2, 0.75wt% dispersant castor oil is added to the mixed solvent, stirred uniformly and ultrasonic dispersed for 15 min. Among them, the mass ratio of mixed powder (zirconium boride powder and boron oxide powder) to dispersant is 1:0.75, the mass of mixed powder added is fixed, which is determined by solid content, and the amount of dispersant added is determined according to the mixed powder. After determining the amount, add the dispersant first and then add the mixed powder.

[0071] S3, zirconium boride powder and boron oxide powder with a mass ratio of 1:0.01 are weighed and added to the solution prepared in step S2, and then fully stirred and ultrasonic dispersed for 30 min;

[0072] S4, the mixed powder slurry prepared in step S3 is placed in a adjustable high-speed homogenizer with a rotating speed of 14000r / min and stirred for 30 min, so that the powder can be fully and uniformly dispersed.

[0073] S5, the mixed zirconium boride slurry is filtered by a needle type filter membrane filter (organic) with a pore size of 1μm to remove large particles formed by agglomeration in the slurry.

[0074] Example 5,

[0075] A preparation method of a zirconium boride slurry, comprising the following steps:

[0076] S1, a mixed solvent is prepared by measuring ethanol and ethylene glycol in a volume ratio of 1:1, and the mixed solvent is ultrasonically dispersed for 15 min to uniformly mix the two solutions.

[0077] S2, 0.75wt% of ammonium oleate and stearic acid dispersant mixed in a mass ratio of 1:2 is added to the mixed solvent, stirred uniformly and ultrasonically dispersed for 15 min. The mass ratio of the mixed powder (zirconium boride powder and boron oxide powder) to the dispersant is 1:0.75, the mass of the mixed powder added is fixed and determined by the solid content, and the amount of the dispersant added is determined according to the mixed powder. After the amount is determined, the dispersant is added first and then the mixed powder is added.

[0078] S3, zirconium boride powder and boron oxide powder with a mass ratio of 1:0.03 are weighed and added to the solution prepared in step S2, and after being stirred fully, ultrasonic dispersion is performed for 30 min;

[0079] S4, the mixed powder slurry prepared in step S3 is placed under an adjustable high-speed homogenizer with a rotating speed of 14000r / min for stirring for 30 min, so that the powder can be fully and uniformly dispersed.

[0080] S5, the mixed zirconium boride slurry is filtered by using a needle type filter membrane filter (organic) with a pore size of 1μm to remove large particles formed by agglomeration in the slurry.

[0081] Example 6,

[0082] A preparation method of a zirconium boride slurry, comprising the following steps:

[0083] S1, a mixed solvent is prepared by measuring ethanol and ethylene glycol in a volume ratio of 2:1, and the mixed solvent is ultrasonically dispersed for 15 min to uniformly mix the two solutions.

[0084] S2, 0.75wt% of dispersant castor oil is added to the mixed solvent, stirred uniformly and ultrasonically dispersed for 15 min. The mass ratio of the mixed powder (zirconium boride powder and boron oxide powder) to the dispersant is 1:0.75, the mass of the mixed powder added is fixed and determined by the solid content, and the amount of the dispersant added is determined according to the mixed powder. After the amount is determined, the dispersant is added first and then the mixed powder is added.

[0085] S3, zirconium boride powder and boron oxide powder with a mass ratio of 1:0.03 are weighed and added to the solution prepared in step S2, and after being stirred fully, ultrasonic dispersion is performed for 30 min;

[0086] S4, the mixed powder slurry prepared in step S3 is placed into an adjustable high-speed homogenizer with a rotation speed of 14000r / min for stirring for 30min, so that the powder can be fully and uniformly dispersed.

[0087] S5, the mixed zirconium boride slurry is filtered by using a needle type filter membrane filter (organic) with a pore size of 1μm to remove large particles formed by agglomeration in the slurry.

[0088] Example 7,

[0089] A preparation method of a zirconium boride slurry, comprising the following steps:

[0090] S1, a mixed solvent is prepared by measuring ethanol and ethylene glycol in a volume ratio of 3:1, and the mixed solvent is ultrasonically dispersed for 15min to uniformly mix the two solutions.

[0091] S2, 0.75wt% of the dispersant castor oil is added to the mixed solvent, stirred uniformly and ultrasonically dispersed for 15min. Among them, the mass ratio of the mixed powder (zirconium boride powder and boron oxide powder) to the dispersant is 1:0.75, the mass of the mixed powder added is fixed, which is determined by the solid content, and the amount of the dispersant added is determined according to the mixed powder. After determining the amount, add the dispersant first and then add the mixed powder.

[0092] S3, zirconium boride powder and boron oxide powder with a mass ratio of 1:0.03 are weighed and added to the solution prepared in step S2, and then stirred and ultrasonically dispersed for 30min;

[0093] S4, the mixed powder slurry prepared in step S3 is placed into an adjustable high-speed homogenizer with a rotation speed of 14000r / min for stirring for 30min, so that the powder can be fully and uniformly dispersed.

[0094] S5, the mixed zirconium boride slurry is filtered by using a needle type filter membrane filter (organic) with a pore size of 1μm to remove large particles formed by agglomeration in the slurry.

[0095] Example 8,

[0096] A preparation method of a zirconium boride slurry, comprising the following steps:

[0097] S1, a mixed solvent is prepared by measuring ethanol, ethylene glycol and glycerol in a volume ratio of 3:1:1, and the mixed solvent is ultrasonically dispersed for 15min to uniformly mix the two solutions.

[0098] S2, 0.75wt% of dispersant castor oil is added in the mixed solvent, stirred uniformly and ultrasonic dispersed for 15min. Among them, the mass ratio of mixed powder (zirconium boride powder and boron oxide powder) and dispersant is 1:0.75, the mass of mixed powder added is fixed, which is determined by solid content, and the amount of dispersant added is determined according to the mixed powder, and the dispersant is added first and then the mixed powder is added.

[0099] S3, zirconium boride powder and boron oxide powder with a mass ratio of 1:0.03 are weighed and added to the solution prepared in step S2, and after being stirred fully, ultrasonic dispersion is carried out for 30min;

[0100] S4, the mixed powder slurry prepared in step S3 is placed under the adjustable high-speed homogenizer with a rotating speed of 14000r / min for stirring for 30min, so that the powder can be fully and uniformly dispersed.

[0101] S5, the mixed zirconium boride slurry is filtered by using a needle type filter membrane filter (organic) with a pore size of 1μm, so as to remove large particles formed by agglomeration in the slurry.

[0102] Example 9,

[0103] A preparation method of zirconium boride slurry comprises the following steps:

[0104] S1, ethanol and ethylene glycol with a volume ratio of 3:1 are measured and prepared into a mixed solvent, and the mixed solvent is ultrasonic dispersed for 10min, so as to uniformly mix the two solutions.

[0105] S2, 1wt% of dispersant castor oil is added in the mixed solvent, stirred uniformly and ultrasonic dispersed for 10min.

[0106] S3, zirconium boride powder and boron oxide powder with a mass ratio of 1:0.03 are weighed and added to the solution prepared in step S2, and after being stirred fully, ultrasonic dispersion is carried out for 25min;

[0107] S4, the mixed slurry prepared in step S3 is placed under the adjustable high-speed homogenizer with a rotating speed of 13000r / min for stirring for 25min, so that the powder can be fully and uniformly dispersed.

[0108] S5, the mixed zirconium boride slurry is filtered by using a needle type filter membrane filter (organic) with a pore size of 1μm, so as to remove large particles formed by agglomeration in the slurry.

[0109] The application further provides a zirconium boride film, which is prepared from the zirconium boride slurry prepared by the above preparation method.

[0110] The preparation method of the zirconium boride film comprises the following steps:

[0111] Step 1, select a non-sintered dense ceramic material as the printing substrate, the sintering temperature of the ceramic substrate is 1100℃, and the substrate is surface treated;

[0112] Step 2, print a zirconium boride film sample on the substrate using the zirconium boride slurry as the raw material;

[0113] Step 3, place the printed sample in an oven for drying, set the oven temperature to 60-80℃, and the time is 30min;

[0114] Step 4, perform photon sintering on the dried sample to obtain a zirconium boride film.

[0115] Preferably, the ceramic substrate includes a thin film ceramic substrate (TFC), a thick film printed ceramic substrate (TPC), and a direct bonded copper ceramic substrate (DBC); the thin film ceramic substrate is a ceramic substrate prepared by thin film technology, which has high thermal conductivity and heat resistance. The thick film printed ceramic substrate is a ceramic substrate prepared by thick film printing technology, which has good mechanical strength and thermal stability. The direct bonded copper ceramic substrate combines the copper layer with the ceramic substrate by direct bonding technology, which has high thermal conductivity and electrical conductivity.

[0116] Example 10,

[0117] A method for preparing a zirconium boride film, comprising the following steps:

[0118] Step 1, select a non-sintered dense ceramic material as the printing substrate, the sintering temperature of the ceramic substrate is 1100℃, and the printing substrate is surface treated: use sodium hydroxide (NaOH) solution to clean the substrate in an ultrasonic instrument for 10min, and then clean it with deionized water.

[0119] Step 2, draw a model and import it into the corresponding software, print a zirconium boride film on the substrate by inkjet printing, as shown in Figure 1 .

[0120] Step 3, place the printed sample in an oven for drying, set the oven temperature to 60℃, and the time is 30min.

[0121] Step 4, use a high-intensity pulsed photon sintering test bench to perform photon sintering on the dried sample, adjust the distance between the sample and the light-emitting lamp tube to 2cm, set the total energy density to 20J / cm 2 , adjust the irradiation time to 2ms.

[0122] Step 5, observe the prepared sample under a scanning electron microscope, as shown in Figure 2 and Figure 3 .

[0123] Example 11,

[0124] A method for preparing a zirconium boride film, comprising the following steps:

[0125] Step 1, selecting a non-sintered dense ceramic material as a printing substrate, the sintering temperature of the ceramic substrate being 1100℃, and performing surface treatment on the printing substrate: cleaning the substrate in an ultrasonic instrument using acetone, methanol and deionized water for 10 min, and then cleaning the substrate with an isopropanol solution for 8 min.

[0126] Step 2, drawing a model and importing it into corresponding software, and printing a zirconium boride film on the substrate by using an inkjet printing method.

[0127] Step 3, placing the printed sample into an oven for drying, setting the oven temperature to 60℃, and the time to 30 min.

[0128] Step 4, using a strong pulsed light sintering test bench to sinter the dried sample, adjusting the distance between the sample and the light-emitting lamp tube to 2 cm, setting the total energy density to 40 J / cm 2 , adjusting the irradiation time to 2 ms, and performing photon sintering.

[0129] Step 5, observing the prepared sample under a scanning electron microscope, as shown in Figure 4 .

[0130] Example 12,

[0131] A method for preparing a zirconium boride film, comprising the following steps:

[0132] Step 1, selecting a non-sintered dense ceramic material as a printing substrate, the sintering temperature of the ceramic substrate being 1100℃, and performing surface treatment on the printing substrate: cleaning the substrate in an ultrasonic instrument using acetone, methanol and deionized water for 10 min, and then cleaning the substrate with an isopropanol solution for 8 min.

[0133] Step 2, drawing a model and importing it into corresponding software, and printing a zirconium boride film on the substrate by using an inkjet printing method.

[0134] Step 3, placing the printed sample into an oven for drying, setting the oven temperature to 60℃, and the time to 30 min.

[0135] Step 4, using a strong pulsed light sintering test bench to sinter the dried sample, adjusting the distance between the sample and the light-emitting lamp tube to 2 cm, setting the total energy density to 40 J / cm 2 , adjusting the irradiation time to 2 ms, and performing photon sintering.

[0136] Step 5, observing the prepared sample under a scanning electron microscope, as shown in Figure 5 and Figure 6 .

[0137] Example 13,

[0138] A method for preparing a zirconium boride film comprises the following steps:

[0139] Step 1: Select unsintered dense ceramic material as the printing substrate. The sintering temperature of the ceramic substrate is 1100℃, and the printed substrate is surface treated by UV / O 3 Clean the substrate with the detergent for 10 minutes.

[0140] Step 2: Draw the model and import it into the corresponding software, and use the inkjet printing method to print the zirconium boride film on the substrate.

[0141] Step 3: Place the printed sample in an oven for drying. The oven temperature is set to 60°C for 30 minutes.

[0142] Step 4: The dried sample is subjected to an intense pulse photon sintering test bench, with the distance between the sample and the light-emitting lamp adjusted to 4 cm, and the total energy density set to 40 J / cm 2 , adjust the irradiation time to 4ms and perform photon sintering.

[0143] The above embodiments are intended only to illustrate the design concepts and features of the present invention. Their purpose is to enable those skilled in the art to understand the contents of the present invention and implement them accordingly. The scope of protection of the present invention is not limited to the above embodiments. Therefore, any equivalent changes or modifications made based on the principles and design concepts disclosed in the present invention are within the scope of protection of the present invention.

Claims

1. A zirconium boride film, characterized in that: The preparation method of zirconium boride slurry comprises the following steps: (1) Preparation of organic solvent: The organic solvent is any one or more of ethanol, ethylene glycol, and glycerol mixed in any mass ratio and subjected to ultrasonic dispersion; (2) adding 0.5-1.5 wt% of a dispersant to an organic solvent, wherein the dispersant is any one or more of ammonium oleate, stearic acid, triolein, and castor oil, mixed in any mass ratio, stirred evenly, and subjected to ultrasonic dispersion; (3) Weigh zirconium boride powder and boron oxide powder in a mass ratio of 1:0.01-0.05, add them to the solution prepared in step (2), stir thoroughly and then perform ultrasonic dispersion, the solid phase content is 5vol%-10vol%; (4) The mixed slurry prepared in step (3) was placed in a homogenizer at a speed of 13000-14000 r / min and stirred for 30-60 min to ensure that the powder was fully and evenly dispersed; (5) Filter out large particles formed by agglomeration with a particle size greater than 1 μm to obtain zirconium boride slurry; The method for preparing the zirconium boride film comprises the following steps: Step 1: Select an unsintered dense ceramic material as the printing substrate and perform surface treatment on the substrate; Step 2, using the zirconium boride slurry as a raw material, printing a zirconium boride thin film sample on a substrate; Step 3: Place the printed sample in an oven for drying; Step 4: Photon sintering the dried sample to obtain a zirconium boride film.

2. The zirconium boride film according to claim 1, characterized in that: In the step (1), the organic solvent is a mixed solvent of ethanol, ethylene glycol and glycerol in a volume ratio of 3:1:

1.

3. The zirconium boride film according to claim 1, characterized in that: In the step (2), the dispersant is a mixture of ammonium oleate and stearic acid in a mass ratio of 1:

2.

4. The zirconium boride film according to claim 1, characterized in that: In the step (3), the average particle size of the zirconium boride powder is 100 nm.

5. The zirconium boride film according to claim 1, characterized in that: In the steps (1) and (2), the ultrasonic dispersion time is 10 to 15 minutes, and in the step (3), the ultrasonic dispersion time is 25 to 30 minutes.

6. The zirconium boride film according to claim 1, characterized in that: The sintering temperature of the ceramic substrate is 1100°C; the oven temperature is set at 60~80°C, and the sintering time is 30 minutes.

7. The zirconium boride film according to claim 1, characterized in that: The printing of the zirconium boride film on the substrate specifically comprises: drawing a film model and importing it into corresponding software, and printing the zirconium boride film on the substrate using an inkjet printing method.

8. The zirconium boride film according to claim 1, characterized in that: The photon sintering is specifically performed as follows: the dried sample is subjected to an intense pulse photon sintering test bench, the distance between the sample and the light-emitting lamp is adjusted to 2-4 cm, and the total energy density is set to 20-40 J / cm 2 , adjust the irradiation time to 2-5ms and perform photon sintering.

9. The zirconium boride film according to claim 1, characterized in that: The surface treatment of the substrate is specifically performed as follows: using acetone, methanol and deionized water to clean the substrate in an ultrasonic instrument for 5 to 10 minutes, and then cleaning the substrate with an isopropyl alcohol solution for 5 to 10 minutes; Alternatively, use sodium hydroxide solution to clean the substrate for 10 to 20 minutes, and then rinse with deionized water; Alternatively, clean the substrate with deionized water in an ultrasonic bath for 10 to 20 minutes; Or use UV / O 3 Clean the substrate for 10 to 20 minutes.

Images