CN113044846B - Process for producing high-purity hafnium silicide by self-propagating method - Google Patents
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Abstract
A process for producing high-purity hafnium silicide by a self-propagating method comprises the steps of adding a binder into hafnium oxide and graphite powder, putting the mixture into a vacuum ball mill, mixing the materials, pressing the mixture into a round cake by an oil press, and putting the round cake into a graphite crucible of a vacuum resistance sintering furnace; vacuumizing to start temperature rise reaction, and after the reaction is finished, stopping power and reducing the temperature along with the furnace to obtain high-purity hafnium; adding sodium nitrate and an adhesive into high-purity hafnium and silicon powder, putting the mixture into a vacuum ball mill, carrying out ball milling and mixing under the protection of argon, pressing the mixture into a round cake by an oil press, putting the round cake into a graphite crucible in a vacuum self-propagating furnace, piling the round cakes layer by layer into a cone shape, putting magnesium powder as an ignition agent, vacuumizing, heating a tungsten wire to ignite the magnesium powder, gradually igniting all the round cakes through heat transfer to carry out self-propagating reaction, and cooling along with the furnace after the self-propagating reaction is finished to obtain the high-purity hafnium silicide. The advantages are that: the process conditions are simple and controllable, the high-cost production process of simple substance synthesis is avoided, the product purity is high, and the large-scale industrial production can be realized.
Description
Technical Field
The invention relates to a process for producing high-purity hafnium silicide by a self-propagating method.
Background
Hafnium silicide is a transition metal silicide, is a refractory intermetallic compound, and is successfully applied to the fields of complementary metal oxide semiconductor elements, thin film coatings, bulk structure components, electric heating elements, thermoelectric materials, photovoltaic materials and the like due to unique physical and chemical properties of the transition metal silicide. The nano material shows special electrical, magnetic and thermoelectric properties, and even has potential application value in the field of catalysis. However, the conventional preparation methods such as metallurgical method or physical method cannot satisfy the preparation of transition metal silicide. Therefore, the search for a simple, controllable and generally applicable preparation method has very important significance for the wide application of the transition metal silicide material.
At present, the production of hafnium silicide mainly comprises the direct combination of simple substance hafnium and simple substance silicon, and the production process has too high production cost, no market competitiveness in price, and the characteristic that silicon is volatile at high temperature, so that the purity and quality of the produced hafnium silicide finished product are uneven, and the market share is low.
Disclosure of Invention
The invention provides a process for producing high-purity hafnium silicide by a self-propagating method, which has the advantages of low cost, high product purity, controllable process and large-scale industrial production.
The technical scheme of the invention is as follows:
a process for producing high-purity hafnium silicide by a self-propagating method comprises the following specific steps:
(1) weighing hafnium oxide and graphite powder according to a molar ratio of 1:2, adding an adhesive, putting into a 10L vacuum ball mill, charging 4kg-6kg each time, and mixing for 15 hours; weighing the mixed material according to 1kg per part, pressing into a round cake by a 400t oil press under 20-25MPa, and then loading into a graphite crucible of a vacuum resistance sintering furnace; vacuumizing to 5Pa-8Pa, starting to heat up, keeping the temperature at 80kw, keeping the temperature at 700 ℃ for 2 hours, discharging moisture of the materials, and keeping the vacuum degree at 5Pa-8Pa during the heat preservation period; continuing to heat, wherein the heating power is 100kw, the materials begin to react when the temperature rises to 1650 ℃, and the vacuum pump runs quickly to discharge a large amount of generated gas; keeping the temperature for 6 hours, wherein the vacuum degree is kept between 20Pa and 30Pa during the heat preservation period; continuously heating with the heating power of 130kw to 1900 ℃, keeping the temperature for 5 hours, keeping the vacuum degree at 3-5 Pa during the heat preservation period, and after the reaction is finished, cutting off the power and cooling along with the furnace to obtain the high-purity hafnium;
(2) weighing the high-purity hafnium and the silicon powder obtained in the step (1) according to a molar ratio of 1:2, adding sodium nitrate and a bonding agent, adding 35g of sodium nitrate into each kilogram of the high-purity hafnium and the silicon powder according to the total weight of the high-purity hafnium and the silicon powder, putting the mixture into a 20L vacuum ball mill, feeding 10kg of the mixture each time, ball-milling and mixing the materials for 30 hours under the protection of argon, weighing 500g of the mixture each time, pressing the mixture into a round cake by using a 200 ton oil press under the pressure of 15MPa, putting the round cake into a graphite crucible in a vacuum self-propagating furnace, piling the round cakes layer by layer into a cone, feeding 20kg to 30 kg of the round cake each time, putting 50g of magnesium powder as an ignition agent at the top, vacuumizing to 1Pa-3Pa, heating the mixture to a temperature of 3kw-5kw, heating a tungsten filament to 700 ℃ -800 ℃, igniting the magnesium powder, igniting all the round cakes through heat transfer, and heating the round cakes to a temperature of 1600 ℃ -1650 ℃, and after the self-propagating reaction is finished, cooling along with the furnace to obtain the high-purity hafnium silicide.
Furthermore, the purity of the hafnium oxide powder is 99.5%, and the granularity is 325 meshes; the purity of the graphite powder is 99.99 percent, and the granularity is 325 meshes; the purity of the sodium nitrate is 99.9 percent, and the granularity is 200 meshes; the purity of the magnesium powder is 99.5 percent, and the granularity is 325 meshes; the purity of the silicon powder is 99.99 percent, and the granularity is 500 meshes.
Further, the adhesive added in the step (1) is carboxymethyl cellulose, the adding amount of the adhesive is 5g per kg of the total weight of the hafnium oxide and the graphite powder. And (3) the adhesive in the step (2) is carboxymethyl cellulose, the addition amount of the adhesive is 5g based on the total weight of the high-purity hafnium and the silicon powder, and each kilogram of the high-purity hafnium and the silicon powder is added with the adhesive.
By adopting the technical scheme, the method has the following beneficial effects:
the method comprises the steps of sintering high-purity hafnium by utilizing hafnium oxide and graphite, sintering the high-purity hafnium silicide by utilizing the high-purity hafnium and simple substance silicon through a self-propagating reaction, and completing the steps through two steps, thereby realizing low cost, simple and controllable process conditions, getting rid of a high-cost production process of synthesizing the simple substance, and filling the domestic blank of low cost, easy process operation and industrial production. And sodium nitrate is added in the self-propagating reaction process, so that the heat energy of the self-propagating reaction meets the requirement of raw material reaction, the product purity is high, the process is controllable, and the large-scale industrial production can be realized.
Drawings
FIG. 1 is an electron microscope image of hafnium silicide produced by the present invention;
FIG. 2 is an X-ray diffraction pattern of hafnium silicide produced according to the present invention.
Detailed Description
The present invention will be explained in more detail by the following examples, but the present invention is not limited to the following examples.
The raw material requirements are as follows: the purity of the hafnium oxide powder is 99.5 percent, and the granularity is 325 meshes; the purity of the graphite powder is 99.99 percent, and the granularity is 325 meshes; the purity of the silicon powder is 99.99 percent, and the granularity is 500 meshes; the purity of the sodium nitrate is 99.9 percent, and the granularity is 200 meshes; the purity of the magnesium powder is 99.5 percent, and the granularity is 325 meshes;
(1) adding 111g of carboxymethyl cellulose serving as a binder into 20kg of hafnium oxide and 2.27kg of graphite powder (the molar ratio of the hafnium oxide to the graphite powder is 1:2), putting the mixture into a 10L vacuum ball mill, charging 4kg-6kg of the binder each time, and mixing for 15 hours; weighing the mixed material according to 1kg per part, pressing into a round cake by a 400t oil press under 20-25MPa, and then putting into a graphite crucible of a vacuum resistance sintering furnace; vacuumizing to 5Pa-8Pa, starting to heat up, keeping the temperature at 80kw, keeping the temperature at 700 ℃ for 2 hours, discharging moisture of the materials, and keeping the vacuum degree at 5Pa-8Pa during the heat preservation period; continuing to heat, wherein the heating power is 100kw, the temperature is increased to 1650 ℃, the materials begin to react, the vacuum pump runs in an accelerating way to discharge a large amount of generated gas, the temperature is kept for 6 hours, and the vacuum degree is kept at 20-30 Pa during the heat preservation period; continuously heating with the heating power of 130kw to 1900 ℃, keeping the temperature for 5 hours, keeping the vacuum degree at 3-5 Pa during the heat preservation period, and after the reaction is finished, cutting off the power and cooling along with the furnace to obtain the high-purity hafnium;
(2) adding 777g of sodium nitrate and 111g of binder carboxymethyl cellulose into 16.88kg of high-purity hafnium obtained in the step (1) and 5.31kg of silicon powder (the molar ratio is 1:2), putting the mixture into a 20L vacuum ball mill, feeding 10kg of the mixture each time, ball-milling and mixing the mixture for 30 hours under the protection of argon, weighing 500g of the mixture according to each part, pressing the mixture into a round cake under the pressure of 15MPa by using a 200-ton oil press, putting the round cake into a graphite crucible in a 200-kg vacuum self-propagating furnace, stacking the round cakes layer by layer to form a cone, gradually reducing the number of the round cakes from the bottom layer to the top layer when stacking, putting 20kg to 30 kg of the round cakes each time, putting 50g of magnesium powder as an ignition agent at the top, vacuumizing to 1Pa-3Pa, heating the mixture to a temperature of 3kw-5kw, heating a tungsten filament to 700 ℃ -800 ℃, igniting the magnesium powder, igniting all the round cakes through heat transfer, heating the temperature to 1650 ℃ -1650 ℃, fully carrying out a combination reaction, cooling along with the furnace after the self-propagating reaction is finished, and obtaining the high-purity hafnium silicide, wherein the X-ray diffraction pattern of the product is shown in figure 1.
Example 1
The raw material requirements are as follows: the purity of the hafnium oxide powder is 99.5 percent, and the granularity is 325 meshes; the purity of the graphite powder is 99.99 percent, and the granularity is 325 meshes; the purity of the sodium nitrate is 99.9 percent, and the granularity is 200 meshes; the purity of the magnesium powder is 99.5 percent, and the granularity is 325 meshes; the purity of the silicon powder is 99.99 percent, and the granularity is 500 meshes;
(1) adding 111g of carboxymethyl cellulose serving as a binder into 20kg of hafnium oxide and 2.27kg of graphite powder (the molar ratio of the hafnium oxide to the graphite powder is 1:2), putting the mixture into a 10L vacuum ball mill, charging 4kg of the mixture every time, and mixing the materials for 15 hours; weighing the mixed material according to 1kg per part, pressing the mixed material into a round cake by a 400t oil press under 20MPa, and then putting the round cake into a graphite crucible of a vacuum resistance sintering furnace; vacuumizing to 5Pa-8Pa, starting heating, keeping the temperature at 80kw, keeping the temperature at 700 ℃ for 2 hours, discharging moisture of the material, and keeping the vacuum degree at 5Pa-8Pa during the heat preservation period; continuously heating, wherein the heating power is 100kw, the materials start to react when the temperature is increased to 1650 ℃, and a vacuum pump runs in an accelerated manner to discharge a large amount of generated gas; keeping the temperature for 6 hours, wherein the vacuum degree is kept between 20Pa and 30Pa during the heat preservation period; continuously heating with the heating power of 130kw to 1900 ℃, keeping the temperature for 5 hours, keeping the vacuum degree at 3-5 Pa during the heat preservation period, and after the reaction is finished, cutting off the power and cooling along with the furnace to obtain high-purity hafnium;
(2) adding 777g of sodium nitrate and 111g of carboxymethyl cellulose serving as a binder into 16.88kg of high-purity hafnium obtained in the step (1) and 5.31kg of silicon powder (the molar ratio is 1:2), putting the mixture into a 20L vacuum ball mill, feeding 10kg of the mixture each time, ball-milling and mixing the mixture for 30 hours under the protection of argon, weighing 500g of the mixture, pressing the mixture into round cakes by using a 200-ton oil press under the pressure of 15MPa, putting the round cakes into a graphite crucible in a vacuum self-propagating furnace, stacking the round cakes layer by layer to form a cone, wherein when the round cakes are stacked layer by layer, the number of the round cakes is gradually decreased from the bottom layer to the top layer, the top layer is 1, and the difference between two adjacent layers is 1. Each time, the loading amount is 21 kilograms, 50 grams of magnesium powder is put at the top as an igniter, the vacuum pumping is carried out until the pressure is 1Pa-3Pa, the temperature is raised, the heating power is 3kw, the tungsten wire is heated to 700 ℃ -800 ℃, the magnesium powder is ignited, all round cakes are ignited through heat transfer, the temperature reaches 1600 ℃, the combination reaction is fully carried out, and the temperature is reduced along with the furnace after the self-propagating reaction is finished, so that the high-purity hafnium silicide is obtained. The electron micrograph of the produced hafnium silicide is shown in fig. 1, and it can be seen from fig. 2 that the electron micrograph is substantially consistent with the standard card of hafnium silicide, and the sample produced by the method has no obvious impurity.
Example 2
The raw material requirements are as follows: the purity of the hafnium oxide powder is 99.5 percent, and the granularity is 325 meshes; the purity of the graphite powder is 99.99 percent, and the granularity is 325 meshes; the purity of the sodium nitrate is 99.9 percent, and the granularity is 200 meshes; the purity of the magnesium powder is 99.5 percent, and the granularity is 325 meshes; the purity of the silicon powder is 99.99 percent, and the granularity is 500 meshes;
(1) adding 111g of carboxymethyl cellulose serving as a binder into 20kg of hafnium oxide and 2.27kg of graphite powder (the molar ratio of the hafnium oxide to the graphite powder is 1:2), putting the mixture into a 10L vacuum ball mill, charging 5kg of the mixture every time, and mixing the materials for 15 hours; weighing the mixed material according to 1kg per part, pressing the mixed material into a round cake by a 400t oil press under 22MPa, and then loading the round cake into a graphite crucible of a vacuum resistance sintering furnace; vacuumizing to 5Pa-8Pa, starting heating, keeping the temperature at 80kw, keeping the temperature at 700 ℃ for 2 hours, discharging moisture of the material, and keeping the vacuum degree at 5Pa-8Pa during the heat preservation period; continuing to heat, wherein the heating power is 100kw, the materials begin to react when the temperature rises to 1650 ℃, and the vacuum pump runs quickly to discharge a large amount of generated gas; keeping the temperature for 6 hours, wherein the vacuum degree is kept between 20Pa and 30Pa during the heat preservation period; continuously heating with the heating power of 130kw to 1900 ℃, keeping the temperature for 5 hours, keeping the vacuum degree at 3-5 Pa during the heat preservation period, and after the reaction is finished, cutting off the power and cooling along with the furnace to obtain the high-purity hafnium;
(2) adding 777g of sodium nitrate and 111g of carboxymethyl cellulose serving as a binder into 16.88kg of high-purity hafnium obtained in the step (1) and 5.31kg of silicon powder (the molar ratio is 1:2), putting the mixture into a 20L vacuum ball mill, feeding 10kg of the mixture each time, ball-milling and mixing the mixture for 30 hours under the protection of argon, weighing 500g of the mixture, pressing the mixture into round cakes by using a 200-ton oil press under the pressure of 15MPa, putting the round cakes into a graphite crucible in a vacuum self-propagating furnace, stacking the round cakes layer by layer to form a cone, wherein when the round cakes are stacked layer by layer, the number of the round cakes is gradually decreased from the bottom layer to the top layer, the top layer is 1, and the difference between two adjacent layers is 1. Each time, the loading amount is 28 kilograms, 50 grams of magnesium powder is put at the top as an igniter, the vacuum pumping is carried out until the pressure is 1Pa-3Pa, the temperature is raised, the heating power is 4kw, the tungsten wire is heated to 700 ℃ -800 ℃, the magnesium powder is ignited, all round cakes are ignited through heat transfer, the temperature reaches 1628 ℃, the combination reaction is fully carried out, and the temperature is reduced along with the furnace after the self-propagating reaction is finished, so that the high-purity hafnium silicide is obtained. The electron micrograph of the produced hafnium silicide is shown in fig. 1, and it can be seen from fig. 2 that the electron micrograph is substantially consistent with the standard card of hafnium silicide, and the sample produced by the method has no obvious impurity.
Example 3
The raw material requirements are as follows: the purity of the hafnium oxide powder is 99.5 percent, and the granularity is 325 meshes; the purity of the graphite powder is 99.99 percent, and the granularity is 325 meshes; the purity of the sodium nitrate is 99.9 percent, and the granularity is 200 meshes; the purity of the magnesium powder is 99.5 percent, and the granularity is 325 meshes; the purity of the silicon powder is 99.99 percent, and the granularity is 500 meshes;
(1) adding 111g of carboxymethyl cellulose serving as a binder into 20kg of hafnium oxide and 2.27kg of graphite powder (the molar ratio of the hafnium oxide to the graphite powder is 1:2), putting the mixture into a 10L vacuum ball mill, charging 6kg of the mixture each time, and mixing the materials for 15 hours; weighing the mixed material according to 1kg per part, pressing the mixed material into a round cake by a 400t oil press under 25MPa, and then putting the round cake into a graphite crucible of a vacuum resistance sintering furnace; vacuumizing to 5Pa-8Pa, starting heating, keeping the temperature at 80kw, keeping the temperature at 700 ℃ for 2 hours, discharging moisture of the material, and keeping the vacuum degree at 5Pa-8Pa during the heat preservation period; continuing to heat, wherein the heating power is 100kw, the materials begin to react when the temperature rises to 1650 ℃, and the vacuum pump runs quickly to discharge a large amount of generated gas; keeping the temperature for 6 hours, wherein the vacuum degree is kept between 20Pa and 30Pa during the heat preservation period; continuously heating with the heating power of 130kw to 1900 ℃, keeping the temperature for 5 hours, keeping the vacuum degree at 3-5 Pa during the heat preservation period, and after the reaction is finished, cutting off the power and cooling along with the furnace to obtain the high-purity hafnium;
(2) adding 777g of sodium nitrate and 111g of carboxymethyl cellulose serving as a binder into 16.88kg of high-purity hafnium obtained in the step (1) and 5.31kg of silicon powder (the molar ratio is 1:2), putting the mixture into a 20L vacuum ball mill, feeding 10kg of the mixture each time, ball-milling and mixing the mixture for 30 hours under the protection of argon, weighing 500g of the mixture, pressing the mixture into round cakes by using a 200-ton oil press under the pressure of 15MPa, putting the round cakes into a graphite crucible in a vacuum self-propagating furnace, stacking the round cakes layer by layer to form a cone, wherein when the round cakes are stacked layer by layer, the number of the round cakes is gradually decreased from the bottom layer to the top layer, the top layer is 1, and the difference between two adjacent layers is 1. Each time, the loading amount is 28 kilograms, 50 grams of magnesium powder is put at the top as an igniter, the vacuum pumping is carried out until the pressure is 1Pa-3Pa, the temperature is raised, the heating power is 5kw, the tungsten wire is heated to 700 ℃ -800 ℃, the magnesium powder is ignited, all round cakes are ignited through heat transfer, the temperature reaches 1650 ℃, the combination reaction is fully carried out, and the temperature is reduced along with the furnace after the self-propagating reaction is finished, so that the high-purity hafnium silicide is obtained. The electron micrograph of the produced hafnium silicide is shown in fig. 1, and it can be seen from fig. 2 that the electron micrograph is substantially consistent with the standard card of hafnium silicide, and the sample produced by the method has no obvious impurity.
The present invention is not limited to the above embodiments, but various modifications and changes can be made by those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (2)
1. A process for producing high-purity hafnium silicide by a self-propagating method is characterized by comprising the following steps:
the method comprises the following specific steps:
(1) weighing hafnium oxide and graphite powder according to a molar ratio of 1:2, adding an adhesive, putting into a 10L vacuum ball mill, charging 4kg-6kg each time, and mixing for 15 hours; weighing the mixed material according to 1kg per part, pressing into a round cake by a 400t oil press under 20-25MPa, and then loading into a graphite crucible of a vacuum resistance sintering furnace; vacuumizing to 5Pa-8Pa, starting to heat up, keeping the temperature at 80kw, keeping the temperature at 700 ℃ for 2 hours, discharging moisture of the materials, and keeping the vacuum degree at 5Pa-8Pa during the heat preservation period; continuously heating, wherein the heating power is 100kw, the temperature is increased to 1650 ℃, the materials start to react, keeping the temperature for 6 hours, and the vacuum degree is kept between 20Pa and 30Pa during the heat preservation period; continuously heating with the heating power of 130kw to 1900 ℃, keeping the temperature for 5 hours, keeping the vacuum degree at 3-5 Pa during the heat preservation period, and after the reaction is finished, cutting off the power and cooling along with the furnace to obtain the high-purity hafnium;
(2) weighing the high-purity hafnium and the silicon powder obtained in the step (1) according to a molar ratio of 1:2, adding sodium nitrate and a binder, wherein the adding amount of the sodium nitrate is 35g per kg of the high-purity hafnium and the silicon powder according to the total weight of the high-purity hafnium and the silicon powder, putting the mixture into a 20L vacuum ball mill, and feeding 10kg per time, ball-milling and mixing for 30 hours under the protection of argon, weighing 500g of the mixture in each part after the mixing is finished, pressing the mixture into a round cake under the pressure of 15MPa by a 200-ton oil press, then loading the round cake into a graphite crucible in a vacuum self-propagating furnace, piling the round cakes layer by layer into a cone, filling 20-30 kg of the round cakes each time, putting 50g of magnesium powder as an igniter at the top, vacuumizing to 1-3 Pa, heating to 3-5 kw, heating a tungsten filament to 700-800 ℃, igniting the magnesium powder, igniting all round cakes to perform self-propagating reaction through heat transfer, wherein the temperature reaches 1600-1650 ℃; after the self-propagating reaction is finished, cooling along with the furnace to obtain high-purity hafnium silicide;
the purity of the hafnium oxide powder is 99.5 percent, and the granularity is 325 meshes; the purity of the graphite powder is 99.99 percent, and the granularity is 325 meshes; the purity of the sodium nitrate is 99.9 percent, and the granularity is 200 meshes; the purity of the magnesium powder is 99.5 percent, and the granularity is 325 meshes; the purity of the silicon powder is 99.99%, and the particle size is 500 meshes.
2. The process for producing high purity hafnium silicide by the self-propagating method according to claim 1, wherein:
the adhesive added in the step (1) is carboxymethyl cellulose, the adding amount of the adhesive is based on the total weight of the hafnium oxide and the graphite powder, and 5g of the adhesive is added into each kilogram of the hafnium oxide and the graphite powder; and (3) the adhesive in the step (2) is carboxymethyl cellulose, the addition amount of the adhesive is 5g based on the total weight of the high-purity hafnium and the silicon powder, and each kilogram of the high-purity hafnium and the silicon powder is added with the adhesive.
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