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CN107200578B - A kind of preparation method of Sr2YTaO6 thermal barrier coating material - Google Patents

A kind of preparation method of Sr2YTaO6 thermal barrier coating material Download PDF

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CN107200578B
CN107200578B CN201710358025.2A CN201710358025A CN107200578B CN 107200578 B CN107200578 B CN 107200578B CN 201710358025 A CN201710358025 A CN 201710358025A CN 107200578 B CN107200578 B CN 107200578B
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刘玲
马壮
王英华
柳彦博
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Beijing Institute of Technology BIT
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Abstract

本发明涉及一种Sr2YTaO6热障涂层材料的制备方法，属于新材料领域。所述材料中Y为镧系元素，所述方法为：将干燥原料SrCO3、Y2O3和Ta2O5粉每分钟300转～500转的转速球磨5h～8h；用小于等于0.5h去除无水乙醇，得到干燥的粉体；放入坩埚中以1℃/min～10℃/min的升温速度加热至700℃～900℃，煅烧6h～10h后冷却，得到煅烧后的粉体；在研钵中碾磨，并用250目～300目的筛子筛粉，将筛好的粉体直接煅烧或在模具中进行定型后再煅烧；以1℃/min～10℃/min的升温速度加热至1300℃～1600℃，煅烧8h～12h，煅烧后冷却，得到所述材料。The invention relates to a preparation method of a Sr 2 YTaO 6 thermal barrier coating material, belonging to the field of new materials. Y in the material is a lanthanide element, and the method is as follows: ball-milling the dry raw materials SrCO 3 , Y 2 O 3 and Ta 2 O 5 powder at a rotational speed of 300 to 500 rpm for 5h to 8h; using less than or equal to 0.5h Remove absolute ethanol to obtain dry powder; put it into a crucible and heat it to 700°C to 900°C at a heating rate of 1°C/min to 10°C/min, calcinate for 6h to 10h and then cool to obtain calcined powder; Grind in a mortar, and sieve the powder with a 250-300-mesh sieve. The sieved powder is directly calcined or set in a mold and then calcined; heated at a heating rate of 1°C/min～10°C/min to 1300℃～1600℃, calcination for 8h～12h, and cooling after calcination to obtain the material.

Description

Sr2YTaO6Preparation method of thermal barrier coating material
Technical Field
The invention relates to a Sr2YTaO6A preparation method of a thermal barrier coating material belongs to the field of new materials.
Background
With the continuous development of aviation industry, the service temperature of an aero-engine is continuously increased, and a hot end part material of the aero-engine is required to have better high temperature resistance. As a main high-temperature protective material in the present generation, a thermal barrier coating needs to satisfy specific requirements, such as a high melting point, a high thermal expansion coefficient, a low thermal conductivity, and good high-temperature chemical stability, and also needs to ensure good structural stability during high and low temperature cycling.
The most commonly used thermal barrier coating material at present is Yttria Stabilized Zirconia (YSZ), but when the temperature reaches 1200 ℃, the material undergoes phase change from tetragonal phase to monoclinic phase, which causes 3-5% volume expansion, and the expansion causes problems of cracking, peeling and the like of the coating, finally leading to failure of the coating, so that the coating cannot meet the requirements of the current generation. The development of new thermal barrier coating materials is necessary.
Disclosure of Invention
The invention aims to provide Sr2YTaO6The preparation method of the thermal barrier coating material can finish Sr used for the research of the field of thermal barrier coatings2YTaO6And (4) preparing the material.
In order to achieve the purpose of the invention, the following technical scheme is provided.
Sr2YTaO6The preparation method of the thermal barrier coating material comprises the following steps of: lanthanum (La), cerium (Ce), praseodymium (Pr), neodymium (Nd), promethium (Pm), samarium (Sm), europium (Eu), gadolinium (Gd), terbium (Tb), dysprosium (Dy), holmium (Ho), erbium (Er), thulium (Tm), ytterbium (Yb) or lutetium (Lu), said method comprising the steps of:
(1) placing a ball milling tank with the dry raw materials in a ball mill, adding ball milling beads, using absolute ethyl alcohol as a ball milling medium, and performing ball milling for 5-8 h at a rotating speed of 300-500 r/min to obtain a ball-milled material;
wherein the required raw material is strontium carbonate (SrCO)3) Powder, lanthanide oxide (Y)2O3) Powder and tantalum pentoxide (Ta)2O5) Powder of Y2O3Is La2O3、Ce2O3、Pr2O3、Nd2O3、Pm2O3、Sm2O3、Eu2O3、 Gd2O3、Tb2O3、Dy2O3、Ho2O3、Er2O3、Tm2O3、Yb2O3Or Lu2O3The dosage of the raw materials is proportioned according to a chemical formula; preferably SrCO3The purity of the powder is more than 99.05 percent, Y2O3Purity of powder is above 99.99%, Ta2O5The purity of the powder is more than 99.99 percent.
The mass ratio of the ball milling beads to the raw materials is 4-3: 1.
Due to the moiety Y2O3Is easy to absorb water, preferably Y2O3First, theHeating to 700-900 ℃ at a heating rate of 1-10 ℃/min, calcining for 6-9 h, and cooling to obtain dried Y2O3(ii) a The temperature rise rate is preferably 5 ℃/min.
The preferred ball milling beads are corundum ball milling beads, and consist of large balls with the diameter range of 25 cm-30 cm, medium balls with the diameter range of 15 cm-20 cm and small balls with the diameter range of 5 cm-10 cm, and the mass ratio of the large balls, the medium balls and the small balls is preferably 1:2: 1.
(2) And removing absolute ethyl alcohol from the ball-milled materials by less than or equal to 0.5h to obtain dry powder.
Preferably, the ball-milled material is dried by rotary evaporation by a rotary evaporation instrument, and then the dried material is placed in an oven and dried for 10 to 12 hours at the temperature of between 100 and 150 ℃ to ensure that the absolute ethyl alcohol is completely evaporated to obtain dry powder.
(3) And placing the dried powder in a crucible, heating to 700-900 ℃ at a heating rate of 1-10 ℃/min, calcining for 6-10 h, and cooling to obtain calcined powder.
The temperature rise rate is preferably 5 ℃/min.
(4) Grinding the calcined powder in a mortar, and sieving the powder by using a 250-300-mesh sieve, preferably 300-mesh sieve; directly calcining the screened powder or shaping the powder in a mould in the shape of the required product and then calcining the powder according to the product to be prepared; heating to 1300-1600 ℃ at the heating rate of 1-10 ℃/min, calcining for 8-12 h, and cooling after calcining to obtain the Sr of the invention2YTaO6A thermal barrier coating material.
The temperature rise rate is preferably 5 ℃/min.
Detailed Description
The present invention is further illustrated by the following examples.
In the following examples:
SrCO3the purity of the powder is 99.05 percent, and the La content2O3Purity of powder is 99.99%, Ta2O5The purity of the powder is 99.99 percent and the powder is purchased from the chemical technology company of Rell, Guangdong, Huizhou;
the muffle furnace is LHT04/17 muffle furnace, Nabo fever, Germany;
the ball mill is QM-3SP4 star ball mill, Nanjing university instrument factory;
the rotary steaming instrument is an SENCO rotary steaming instrument, Shanghai Shensheng science and technology Limited;
the oven is a DHG-9070A oven, Shanghai Pudong Rongfeng scientific instruments Co., Ltd;
the X-ray diffractometer is X' Pert PRO MPD type, PANALYTICAL CORPORATION, the Netherlands;
example 1
Sr2LaTaO6The preparation method of the thermal barrier coating material comprises the following steps:
(1) heating La at a temperature rise rate of 2 ℃/min2O3Heating the mixture to 700 ℃ in a muffle furnace, calcining the mixture for 9 hours, and then cooling the calcined mixture along with the furnace to obtain dry La2O3Powder; weighing the dried raw material SrCO3Powder 24.97g, La2O3Powder 13.78g and Ta2O5Putting 18.69g of powder into a ball milling tank, adding 200g of corundum ball milling beads, wherein the ball milling beads consist of large balls with the diameter of 25cm, medium balls with the diameter of 15cm and small balls with the diameter of 5cm, and the mass ratio of the large balls to the medium balls to the small balls is 1:2: 1; adding absolute ethyl alcohol as a ball milling medium to enable the absolute ethyl alcohol to be over the raw materials and ball milling beads, and placing the mixture in a ball mill to perform ball milling for 6 hours at a rotating speed of 400 revolutions per minute to obtain a ball-milled material.
(2) And (3) performing rotary evaporation drying on the ball-milled material for 10min by using a rotary evaporator until the solvent absolute ethyl alcohol is removed to obtain a rotary evaporation dried material, placing the rotary evaporation dried material in an oven, and drying at 100 ℃ for 12h to ensure that the absolute ethyl alcohol is completely evaporated to obtain dried powder.
(3) And placing the dried powder in a crucible, heating the dried powder to 700 ℃ in a muffle furnace at a heating rate of 5 ℃/min, calcining the powder for 9 hours, and cooling the calcined powder to obtain the calcined powder.
(4) And grinding the calcined powder in a mortar, sieving the powder by using a 300-mesh sieve to obtain powder with the particle size of below 50 mu m, heating the powder to 1300 ℃ in a muffle furnace at the temperature rising speed of 5 ℃/min, calcining the powder for 12h, and cooling the calcined powder along with the furnace to obtain a final product.
The final product obtained in this example was used as a sample for testing, and the results were as follows: the sample is detected by an X-ray diffractometer, and the three strong peaks appear at the positions of 15.295 degrees, 21.958 degrees and 27.116 degrees of theta, and the three strong peaks are matched with Sr in an XRD card2LaTaO6The standard peaks correspond to one another, and other small peaks are basically identical, indicating that the final product is Sr2LaTaO6Is Sr described in the invention2YTaO6A thermal barrier coating material.
Example 2
Sr2LaTaO6The preparation method of the thermal barrier coating material comprises the following steps:
(1) heating La at a temperature rise rate of 5 ℃/min2O3Heating to 800 ℃ in a muffle furnace, calcining for 8h, and cooling with the furnace to obtain dry La2O3(ii) a Weighing the dried raw material SrCO3Powder 24.97g, La2O3Powder 13.78g and Ta2O5Putting 18.69g of powder into a ball milling tank, adding 200g of corundum ball milling beads, wherein the ball milling beads consist of large balls with the diameter of 30cm, medium balls with the diameter of 20cm and small balls with the diameter of 10cm, and the mass ratio of the large balls to the medium balls to the small balls is 1:2: 1; adding absolute ethyl alcohol as a ball milling medium to enable the absolute ethyl alcohol to be over the raw materials and ball milling beads, and placing the mixture in a ball mill to perform ball milling for 6 hours at a rotating speed of 400 revolutions per minute to obtain a ball-milled material.
(2) And (3) performing rotary evaporation drying on the ball-milled material for 12min by using a rotary evaporator until the solvent absolute ethyl alcohol is removed to obtain a rotary evaporation dried material, placing the rotary evaporation dried material in an oven, and drying at 150 ℃ for 10h to ensure that the absolute ethyl alcohol is completely evaporated to obtain dried powder.
(3) And placing the dried powder in a crucible, heating the dried powder to 800 ℃ in a muffle furnace at a heating rate of 5 ℃/min, calcining the powder for 8 hours, and cooling the calcined powder to obtain the calcined powder.
(4) And grinding the calcined powder in a mortar, sieving the powder by using a 300-mesh sieve to obtain powder with the particle size of below 50 mu m, heating the powder to 1600 ℃ in a muffle furnace at the temperature rising speed of 5 ℃/min, calcining for 8h, and cooling the calcined powder along with the furnace to obtain a final product.
The final product obtained in this example was used as a sample for testing, and the results were as follows: detecting the sample by using an X-ray diffractometer, and finding that the sample has three strong peaks at the positions of 15.295 degrees, 21.958 degrees and 27.116 degrees of theta and Sr in an XRD card2LaTaO6The standard peaks correspond to one another, and other small peaks are basically identical, indicating that the final product is Sr2LaTaO6Is Sr described in the invention2YTaO6A thermal barrier coating material.
Example 3
Sr2LaTaO6The preparation method of the thermal barrier coating material comprises the following steps:
(1) heating La at a temperature rise rate of 9 ℃/min2O3Heating to 900 ℃ in a muffle furnace, calcining for 6h, and cooling with the furnace to obtain dry La2O3(ii) a Weighing the dried raw material SrCO3Powder 24.97g, La2O3Powder 13.78g and Ta2O5Putting 18.69g of powder into a ball milling tank, adding 200g of corundum ball milling beads, wherein the ball milling beads consist of large balls with the diameter of 27cm, medium balls with the diameter of 17cm and small balls with the diameter of 7cm, and the mass ratio of the large balls to the medium balls to the small balls is 1:2: 1; adding absolute ethyl alcohol as a ball milling medium to enable the absolute ethyl alcohol to be over the raw materials and ball milling beads, and placing the mixture in a ball mill to perform ball milling for 6 hours at a rotating speed of 400 revolutions per minute to obtain a ball-milled material.
(2) And (3) performing rotary evaporation drying on the ball-milled material for 15min by using a rotary evaporation instrument until the solvent is removed to obtain a rotary evaporation dried material, then placing the rotary evaporation dried material in an oven, and drying at 120 ℃ for 11h to ensure that the absolute ethyl alcohol is completely evaporated to obtain dried powder.
(3) And placing the dried powder in a crucible, heating the dried powder to 900 ℃ in a muffle furnace at a heating rate of 9 ℃/min, calcining the powder for 6 hours, and cooling the calcined powder to obtain the calcined powder.
(4) And grinding the calcined powder in a mortar, sieving the powder by using a 300-mesh sieve to obtain powder with the particle size of below 50 mu m, heating the powder to 1400 ℃ in a muffle furnace at the temperature rising speed of 5 ℃/min, calcining the powder for 10h, and cooling the calcined powder along with the furnace to obtain a final product.
The final product obtained in this example was used as a sample for testing, and the results were as follows: detecting the sample by using an X-ray diffractometer, and finding that the sample has three strong peaks at the positions of 15.295 degrees, 21.958 degrees and 27.116 degrees of theta and Sr in an XRD card2LaTaO6The standard peaks correspond to one another, and other small peaks are basically identical, indicating that the final product is Sr2LaTaO6Is Sr described in the invention2YTaO6A thermal barrier coating material.

Claims (1)

1.一种Sr2YTaO6材料应用于热障涂层，其特征在于：Y为La、Ce、Pr、Nd、Pm、Sm、Eu、Tb、Dy、Ho、Er、Tm、Yb或Lu，所述材料的制备方法步骤如下：1. a kind of Sr 2 YTaO 6 material is applied to thermal barrier coating, it is characterized in that: Y is La, Ce, Pr, Nd, Pm, Sm, Eu, Tb, Dy, Ho, Er, Tm, Yb or Lu, The preparation method steps of the material are as follows: (1)将放置有干燥原料的球磨罐置于球磨机中，加入球磨珠，用无水乙醇作为球磨介质，以每分钟300转～500转的转速球磨5h～8h，得到球磨后的物料；(1) Place the ball mill jar with the dry raw materials in the ball mill, add ball milling beads, use absolute ethanol as the ball milling medium, and perform ball milling at a rotational speed of 300 to 500 rpm for 5h to 8h to obtain the ball-milled material; 原料为SrCO3粉、Y2O3粉和Ta2O5粉，球磨珠与原料的质量比为4～3:1；The raw materials are SrCO 3 powder, Y 2 O 3 powder and Ta 2 O 5 powder, and the mass ratio of ball milling beads to raw materials is 4-3:1; (2)对球磨后的物料用小于等于0.5h去除无水乙醇，得到干燥的粉体；(2) Remove absolute ethanol with less than or equal to 0.5h to the ball-milled material to obtain dry powder; (3)将干燥的粉体放置于坩埚中，以5℃/min的升温速度加热至700℃～900℃，煅烧6h～10h后冷却，得到煅烧后的粉体；(3) The dried powder is placed in a crucible, heated to 700°C to 900°C at a heating rate of 5°C/min, calcined for 6h to 10h and then cooled to obtain calcined powder; (4)将煅烧后的粉体置于研钵中碾磨，并用300目的筛子筛粉，将筛好的粉体直接煅烧或在模具中进行定型后再煅烧；以5℃/mm的升温速度加热至1300℃～1400℃，煅烧8h～12h，煅烧后冷却，得到所述的一种Sr2YTaO6热障涂层材料；(4) The calcined powder is ground in a mortar, and sieved with a 300-mesh sieve, and the sieved powder is directly calcined or shaped in a mold and then calcined; at a heating rate of 5°C/mm Heating to 1300℃～1400℃, calcining for 8h～12h, and cooling after calcination to obtain the Sr 2 YTaO 6 thermal barrier coating material; SrCO3粉的纯度为99.05％以上，Y2O3粉的纯度为99.99％以上，Ta2O5粉的纯度为99.99％以上；The purity of SrCO3 powder is more than 99.05%, the purity of Y2O3 powder is more than 99.99%, and the purity of Ta2O5 powder is more than 99.99%; 步骤(1)中：In step (1): 将Y2O3先以5℃/min的升温速度加热至700℃～900℃煅烧6h～9h后冷却，得到干燥的Y2O3；Y 2 O 3 is first heated to 700° C.～900° C. at a heating rate of 5° C./min, calcined for 6h～9h, and then cooled to obtain dry Y 2 O 3 ; 球磨珠为刚玉球磨珠，由直径范围为25cm～30cm的大球、直径范围为15cm～20cm的中球和直径范围为5cm～10cm的小球组成，大球、中球和小球的质量比为1:2:1；The ball grinding beads are corundum ball grinding beads, which are composed of large balls with a diameter ranging from 25cm to 30cm, medium balls with a diameter ranging from 15cm to 20cm and small balls with a diameter ranging from 5cm to 10cm. is 1:2:1; 步骤(2)中：In step (2): 对球磨后的物料使用旋蒸仪进行旋蒸干燥，再将旋蒸干燥后的物料置于烘箱中，在100℃～150℃烘干10h～12h，保证其中无水乙醇完全蒸发，得到干燥的粉体。Use a rotary evaporator to dry the ball-milled material, and then place the rotary-evaporated and dried material in an oven, and dry it at 100°C to 150°C for 10h to 12h to ensure that the anhydrous ethanol is completely evaporated. powder.
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