CN1569368A - Method for preparing nm-class composite rare earth molybdenum material by sol-gal process - Google Patents
Method for preparing nm-class composite rare earth molybdenum material by sol-gal process Download PDFInfo
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Abstract
The invention discloses an infusible metal material, belonging to compound nanometer material field. Especially relates to a method for using sol-gel method to produce nanometer compound rare earth molybdenum material. The method is, in ammonium molybdate solution, the lemon acid is poured in, and then the rare earth nitrate solution is added into the mixed solution. They are dried in the drying box, and form the dry gel. Then the dry gel is baked in furnace, forms compound of molybdenum trioxide and lanthana or lanthanum hydroxide. Finally, they are reduced for 1.5-2.5 hours under temperature of 400-450deg.C and 800-900deg.C in hydrogen furnace. The reduced compound rare earth lanthana is formed under pressure, and it is heated and baked into shape under high temperature and pressure in hydrogen furnace. The material particle is tiny, the density can reach to 95% of the ideal density, the rare earth oxide exists with nanometer particle, the emitting ability is strong, and it can be used as new negative material.
Description
Technical Field
The invention relates to a refractory metal material, belongs to the field of composite nano materials, and particularly relates to a method for preparing a nano composite rare earth molybdenum material by using sol-gel.
Background
The traditional hot cathode material adopts tungsten-thorium oxide material. The working characteristics are as follows: the working temperature is over 1800 ℃, and the thorium element has radioactivity. The rare earth molybdenum material is prepared by doping a certain amount of rare earth oxide in molybdenum and performing plastic processing, so that the excellent cathode material can be prepared, and has the characteristics of environment friendliness, high toughness and strong emission capability, and the working temperature is below 1500 ℃.
At present, the unit molybdenum lanthanum oxide material is researched at home and abroad. In a japanese patent (JP59-17954) it is mentioned that a lanthanum-molybdenum material is both a structural material and a thermionic emission material. The domestic Beijing industry university starts to comprehensively research the thermionic emission performance of the molybdenum lanthanum oxide material and the related mechanism problem thereof, and makes some progress in the aspects of material preparation, cathode structure and electron emission mechanism research. Their studies were published in the "journal of the university of Industrial Beijing" (volume 27, pp290-293, 2001).
Research on the preparation method of the molybdenum oxide powder is that Nie \31066ofBeijing university of industry, Keren and the like adopt a conventional doping method, namely molybdenum dioxide powder and a lanthanum nitrate solution in a certain proportion are mixed in a solid-liquid manner, stirred, sintered and ground. Reducing to form micron-sized rare earth molybdenum composite powder. The cathode material is prepared by conventional pressing and sintering (see patent CN 1360079A). The presence of nano lanthanum oxide was unexpectedly found in experiments, which were believed to be beneficial for hot cathode emission, but was not further investigated. The problem group of the teaching of the T-bit Jun in the great of the Western-Ann intersection has published the preparation of the nano-composite tungsten-thorium oxide material by the ball milling method on materials letters (pp 2776-2779 in 57 year 2003). The 0-3 type nanometer composite tungsten-thorium oxide is successfully prepared at home and abroad by a vacuum hot pressing method for the first time, the emission performance of the material is obviously improved compared with the conventional emission performance, and the nano rare earth oxide can obviously improve the emission performance of the material. However, iron impurities are inevitably introduced into the tungsten-thorium oxide prepared by the ball milling method, which affects further improvement of the emission performance of the cathode, reduces the processing performance of the material, increases the brittleness of the material, and the use of the material in vacuum is affected by low content of iron impurities.
Disclosure of Invention
The invention aims to provide a method for preparing a nano composite rare earth molybdenum material by using a sol-gel method, which has strong thermionic emission capability, strong ablation resistance capability, fine tissue and good strength plasticity.
The technical scheme of the invention is realized as follows: the method is realized by the following steps:
(1) preparing an ammonium molybdate aqueous solution with the concentration of 17.5-26.1%, adding citric acid with the mass equal to that of ammonium molybdate into the ammonium molybdate aqueous solution, adding lanthanum oxide into nitric acid according to the mass of 1.39-2.97% of ammonium molybdate, wherein the concentration of the nitric acid is 55-70%, and the mass of the nitric acid is 6.95-17.82% of the mass of ammonium molybdate, and preparing a rare earth nitrate aqueous solution; adding the rare earth nitrate aqueous solution into a mixed solution of ammonium molybdate aqueous solution and citric acid, adding nitric acid to adjust the pH to 0.7-3, heating in a stirrer and a water-soluble pot, keeping the constant temperature at 80-90 ℃, evaporating and crystallizing to obtain sol, cooling to room temperature at 23-27 ℃ to obtain gel, drying moisture in a drying oven at the temperature of 100-125 ℃ until the gel turns blue, firing in a muffle furnace at the firing temperature of 400-450 ℃ to obtain molybdenum trioxide and rare earth oxide nano composite powder;
(2) heating and reducing the obtained powder in a hydrogen furnace at the temperature of 400-450 DEG C The reaction is carried out at the temperature of 800-900 DEG C Reacting, and reducing for 1.5-2.5 hours respectively to obtain nano molybdenum-rare earth oxide composite powder;
(3) the reduced composite nano molybdenum-rare earth oxide composite powder is formed by cold pressing under the pressure of 450MPa-550MPa, then is formed by hot pressing in a hydrogen furnace, and is formed by hot pressing sintering under the hot pressing temperature of 1400-1600 ℃ and the pressure of 45MPa-55 MPa.
The ammonium molybdate refers to ammonium dimolybdate or ammonium heptamolybdate.
The utility model discloses utilize the sol-gel method to prepare out the even nanocomposite that the rare earth oxide crystalline grain is littleer that contains, because the existence of nanometer lanthanum oxide is favorable to the hot cathode emission, consequently prepare out the even nanocomposite that the rare earth oxide crystalline grain is littleer with the sol-gel method, the block material is prepared out through the metallurgical method to the nanometer composite powder, and the granularity of rare earth oxide through in the molybdenum substrate of final preparation is less than 90nm, the nanometer composite rare earth molybdenum material of making, the transmitting power is strong.
Detailed Description
The present invention will be described in further detail with reference to the following examples:
the first embodiment is as follows:
88.32 g of ammonium heptamolybdate were weighed out to prepare a 17.5% ammonium heptamolybdate aqueous solution, and 88.32 g of citric acid was weighed out and completely dissolved in the ammonium heptamolybdate aqueous solution. Weighing 1.28 g of lanthanum oxide, completely dissolving the lanthanum oxide in 7ml of nitric acid to prepare a lanthanum nitrate solution, and pouring the prepared lanthanum nitrate solution into an ammonium heptamolybdate aqueous solution; nitric acid was added to adjust the pH to 1.5. Heating to 90 deg.C in water-soluble pot, stirring with electric stirrer, evaporating to obtain sol, and cooling to obtain gel at room temperature. Drying in an oven at 110 ℃. Putting the mixture into a muffle furnace to be burned at 450 ℃. Reducing the burned powder in a hydrogen furnace at 450 ℃ and 850 ℃ in two sections to obtain the molybdenum/lanthanum oxide nano powder. Thencold pressing and forming are carried out under the pressure of 500MPa, and then hot pressing and sintering forming are carried out in a hydrogen furnace at 1500 ℃ and under the pressure of 45 MPa. After the breakdown experiment, the nano molybdenum lanthanum oxide cathode material has many emission points and small ablation degree.
Example two:
85.00 g of ammonium dimolybdate is weighed to prepare an ammonium dimolybdate aqueous solution with the concentration of 18 percent, and 85.00 g of citric acid is weighed and completely dissolved in the ammonium dimolybdate aqueous solution. Weighing 1.36 g of lanthanum oxide, completely dissolving the lanthanum oxide in 8ml of nitric acid to prepare a lanthanum nitrate solution, and then adding the prepared lanthanum nitrate solution into an ammonium dimolybdate aqueous solution; nitric acid was added to adjust the pH to 1.2. Heating to 85 deg.C in water-soluble pot, stirring with electric stirrer, evaporating to obtain sol, and cooling to obtain gel at room temperature. Drying in an oven at 115 ℃. Putting the mixture into a muffle furnace to be burned at the temperature of 420 ℃. And reducing the burned powder in a hydrogen furnace at 420 ℃ and 860 ℃ for two sections to obtain the molybdenum/lanthanum oxide nano powder. Then cold pressing and forming are carried out under 480MPa, and then hot pressing and sintering forming are carried out in a hydrogen furnace at 1450 ℃ and under 50 MPa. After the breakdown experiment, the nano molybdenum lanthanum oxide cathode material has many emission points and small ablation degree.
Example three:
126.96 g of ammonium dimolybdate was weighed out to prepare an ammonium dimolybdate aqueous solution with a concentration of 18.6%, and 126.96 g of citric acid was weighed out and completely dissolved in the ammonium dimolybdate aqueous solution. Weighing 2.3 g of lanthanum oxide, completely dissolving the lanthanum oxide in 13ml of nitric acid to prepare a lanthanum nitrate solution, and then adding the prepared lanthanum nitrate solution into an ammonium dimolybdate aqueous solution; nitric acid was added and the pH was adjusted to 2. Heating to 83 deg.C in water-soluble pot, stirring with electric stirrer, evaporating to obtain sol, and cooling to obtain gel at room temperature. Drying in an oven at 115 ℃. Putting the mixture into a muffle furnace to be burned at 430 ℃. And reducing the burned powder in a hydrogen furnace at 430 ℃ and 870 ℃ in two sections to obtain the molybdenum/lanthanum oxide nano powder. Then cold pressing and forming are carried out under the pressure of 470MPa, and then hot pressing and sintering forming are carried out in a hydrogen furnace at 1550 ℃ and under the pressure of 55 MPa. After the breakdown experiment, the nano molybdenum lanthanum oxide cathode material has many emission points and small ablation degree.
Example four:
176.64 g of ammonium heptamolybdate were weighed out to prepare a 19.2% strength aqueous solution of ammonium heptamolybdate, and 176.64 g of citric acid was weighed out and completely dissolved in the aqueous solution of ammonium heptamolybdate. Weighing 3.5 g of lanthanum oxide, completely dissolving the lanthanum oxide in 20ml of nitric acid to prepare a lanthanum nitrate solution, and then adding the prepared lanthanum nitrate solution into an ammonium heptamolybdate aqueous solution; nitric acid was added and the pH was adjusted to 2.3. Heating to 87 deg.C in water-soluble pot, stirring with electric stirrer, evaporating to obtain sol, and cooling to obtain gel at room temperature. Drying in an oven at 105 ℃. Putting the mixture into a muffle furnace to be burned at the temperature of 410 ℃. And reducing the burned powder in a hydrogen furnace at 435 ℃ and 860 ℃ for two sections to obtain the molybdenum/lanthanum oxide nano powder. Then cold pressing and forming are carried out under the pressure of 520MPa, and then hot pressing and sintering forming are carried out in a hydrogen furnace at the temperature of 1570 ℃ under the pressure of 60 MPa. After the breakdown experiment, the nano molybdenum lanthanum oxide cathode material has many emission points and small ablation degree.
Example five:
106.53 g of ammonium heptamolybdate were weighed out to prepare a 19.7% strength aqueous solution of ammonium heptamolybdate, and 106.53 g of citric acid was weighed out and dissolved completely in the aqueous solution of ammonium heptamolybdate. Weighing 2.4 g of lanthanum oxide, completely dissolving the lanthanum oxide in 14ml of nitric acid to prepare a lanthanum nitrate solution, and then adding the prepared lanthanum nitrate solution into an ammonium heptamolybdate aqueous solution; nitric acid was added and the pH was adjusted to 2.5. Adding into water-soluble pot, adding into 90 deg.C, stirring with electric stirrer, evaporating to obtain sol, and cooling at room temperature to obtain gel. Drying in an oven at 105 ℃. Putting the mixture into a muffle furnace to be burned at 415 ℃. Reducing the burned powder in a hydrogen furnace at 500 ℃ and 800 ℃ in two stages to obtain the molybdenum/lanthanum oxide nano powder. Then cold pressing and forming are carried out under 540MPa pressure, and then hot pressing and sintering forming are carried out in a hydrogen furnace at 1560 ℃ under 48MPa pressure. After the breakdown experiment, the nano molybdenum lanthanum oxide cathode material has many emission points and small ablation degree.
Example six:
84.10 g of ammonium dimolybdate were weighed out to prepare a 22.3% strength aqueous solution of ammonium dimolybdate, and 84.10 g of citric acid was weighed out and dissolved completely in the aqueous solution of ammonium dimolybdate. Weighing 2.0 g of lanthanum oxide, completely dissolving the lanthanum oxide in 12ml of nitric acid to prepare a lanthanum nitrate solution, and then adding the prepared lanthanum nitrate solution into an ammonium dimolybdate aqueous solution; adding nitric acid, adjusting pH to 2.7, heating to 85 deg.C in water-soluble pot, stirring with electric stirrer, evaporating to obtain sol, and cooling to obtain gel at room temperature. Drying in an oven at 115 ℃. Putting the mixture into a muffle furnace, and burning the mixture at 435 ℃. Reducing the burned powder in a hydrogen furnace at 445 ℃ and 840 ℃ for two sections to obtain the molybdenum/lanthanum oxide nano powder. Then cold pressing and forming are carried out under the pressure of 470MPa, and then hot pressing and sintering forming are carried out in a hydrogen furnace at 1520 ℃ under the pressure of 45 MPa. After the breakdown experiment, the nano molybdenum lanthanum oxide cathode material has many emission points and small ablation degree.
Example seven:
178.66 g of ammonium heptamolybdate were weighed out to prepare a 23.5% strength aqueous solution of ammonium heptamolybdate, and 178.66 g of citric acid was weighed out and dissolved completely in the aqueous solution of ammonium heptamolybdate. Weighing 4.6 g of lanthanum oxide, completely dissolving the lanthanum oxide in 28ml of nitric acid to prepare a lanthanum nitrate solution, and then adding the prepared lanthanum nitrate solution into an ammonium heptamolybdate aqueous solution; adding nitric acid, adjusting pH to 3, heating to 90 deg.C in water-soluble pot, stirring with electric stirrer, evaporating to obtain sol, and cooling to obtain gel at room temperature. Drying in an oven at 120 ℃. Putting the mixture into a muffle furnace to be burned at 400 ℃. And reducing the burned powder in a hydrogen furnace at 450 ℃ and 830 ℃ in two stages to obtain the molybdenum/lanthanum oxide nanopowder. Then cold pressing and forming are carried out under the pressure of 500MPa, and then hot pressing and sintering forming are carried out in a hydrogen furnace at 1500 ℃ and under the pressure of 50 MPa. After the breakdown experiment, the nano molybdenum lanthanum oxide cathode material has many emission points and small ablation degree.
Example eight:
171.41 g of ammonium dimolybdate were weighed out to prepare a 25.3% strength aqueous solution of ammonium dimolybdate, and 171.41 g of citric acid was weighed out and dissolved completely in the aqueous solution of ammonium dimolybdate. Weighing 4.8 g of lanthanum oxide, completely dissolving the lanthanum oxide in 30ml of nitric acid to prepare a lanthanum nitrate solution, and then adding the prepared lanthanum nitrate solution into an ammonium dimolybdate aqueous solution; adding nitric acid, adjusting pH to 0.9, heating to 85 deg.C in water-soluble pot, stirring with electric stirrer, evaporating to obtain sol, and cooling to obtain gel at room temperature. Drying in an oven at 115 ℃. Putting the mixture into a muffle furnace to be burned at 405 ℃. Reducing the burned powder in a hydrogen furnace at 450 ℃ and 810 ℃ in two stages to obtain the molybdenum/lanthanum oxide nano powder. Then cold pressing and forming are carried out under the pressure of 550MPa, and then hot pressing and sintering forming are carried out in a hydrogen furnace at 1550 ℃ and under the pressure of 55 MPa. After the breakdown experiment, the nano molybdenum lanthanum oxide cathode material has many emission points and small ablation degree.
Example nine:
175.90 g of ammonium heptamolybdate were weighed out to prepare a 26.1% ammonium heptamolybdate aqueous solution, and 175.90 g of citric acid was weighed out and completely dissolved in the ammonium heptamolybdate aqueous solution. Weighing 5.2 g of lanthanumoxide, completely dissolving the lanthanum oxide in 34ml of nitric acid to prepare a lanthanum nitrate solution, and then adding the prepared lanthanum nitrate solution into an ammonium heptamolybdate aqueous solution; adding nitric acid, adjusting pH to 2.5, heating to 90 deg.C in water-soluble pot, stirring with electric stirrer, evaporating to obtain sol, and cooling at room temperature to obtain gel. Drying in an oven at 125 ℃. Putting the mixture into a muffle furnace to be burned at 440 ℃. Reducing the burned powder in a hydrogen furnace at 480 ℃ and 880 ℃ for two sections to obtain the molybdenum/lanthanum oxide nano powder. Then cold pressing and forming are carried out under the pressure of 530MPa, and then hot pressing and sintering forming are carried out in a hydrogen furnace at the temperature of 1560 ℃ and under the pressure of 45 MPa. After the breakdown experiment, the nano molybdenum lanthanum oxide cathode material has many emission points and small ablation degree.
As the ammonium molybdate, various conventional ammonium molybdates can be used.
Claims (2)
1. The method for preparing the nano composite rare earth molybdenum material by using the sol-gel method is characterized by comprising the following steps of:
(1) the concentration of the prepared ammonium molybdate aqueous solution is 17.5-26.1%, and citric acid with the same mass as ammonium molybdate is added into the ammonium molybdate aqueous solution; lanthanum oxide is added into nitric acid according to the mass of 1.39-2.97 percent of that of ammonium molybdate, the concentration of the nitric acid is 55-70 percent, and the mass of the nitric acid is 6.95-17.82 percent of that of the ammonium molybdate, so as to prepare a rare earth nitrate aqueous solution; adding the rare earth nitrate aqueous solution into a mixed solution of ammonium molybdate aqueous solution and citric acid, adding nitric acid to adjust the pH to 0.7-3, heating in a stirrer and a water-soluble pot, keeping the constant temperature at 80-90 ℃, evaporating and crystallizing to obtain sol, cooling to room temperature at 23-27 ℃ to obtain gel, drying moisture in a drying oven at the temperature of 100-125 ℃ until the gel turns blue, firing in a muffle furnace at the firing temperature of 400-450 ℃ to obtain molybdenum trioxide and rare earth oxide nano composite powder;
(2) heating and reducing the obtained powder in a hydrogen furnace at the temperature of 400-450 DEG C The reaction is carried out at the temperature of 800-900 DEG C Reacting, and reducing for 1.5-2.5 hours respectively to obtain nano molybdenum-rare earth oxide composite powder;
(3) the reduced nano molybdenum-rare earth oxide composite powder is formed by cold pressing under the pressure of 450MPa-550MPa, then is formed by hot pressing in a hydrogen furnace, and is formed by hot pressing sintering under the hot pressing temperature of 1400-1600 ℃ and the pressure of 45MPa-55 MPa.
2. The method for preparing a nanocomposite rare earth molybdenum material using a sol-gel process according to claim 1, wherein the ammonium molybdate means ammonium dimolybdate or ammonium heptamolybdate.
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| CN113798504B (en) * | 2021-09-17 | 2023-08-22 | 郑州大学 | Preparation method of rare earth oxide dispersion-reinforced tungsten powder for 3D printing |
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