CN114951676A - Preparation method of high-purity tungsten powder with controlled content of non-metallic elements - Google Patents

Preparation method of high-purity tungsten powder with controlled content of non-metallic elements Download PDF

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CN114951676A
CN114951676A CN202210416378.4A CN202210416378A CN114951676A CN 114951676 A CN114951676 A CN 114951676A CN 202210416378 A CN202210416378 A CN 202210416378A CN 114951676 A CN114951676 A CN 114951676A
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purity
tungsten powder
purity tungsten
apt
content
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CN114951676B (en
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徐国钻
张龙辉
周俊安
羊求民
刘莉
林丽萍
黄春燕
黄月玲
李重义
刘如铁
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Chongyi Zhangyuan Tungsten Co Ltd
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Chongyi Zhangyuan Tungsten Co Ltd
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00—Making metallic powder or suspensions thereof
    • B22F9/16—Making metallic powder or suspensions thereof using chemical processes
    • B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
    • B22F9/20—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from solid metal compounds
    • B22F9/22—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from solid metal compounds using gaseous reductors
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/34—Sputtering
    • C23C14/3407—Cathode assembly for sputtering apparatus, e.g. Target
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P10/00—Technologies related to metal processing
    • Y02P10/20—Recycling

Abstract

The invention relates to a preparation method of high-purity tungsten powder with controlled content of non-metallic elements. In order to effectively reduce the content of non-metal elements (C, H, O, N) in the high-purity tungsten powder, the invention provides a preparation method of the high-purity tungsten powder, which can control the content of the non-metal elements. The invention takes high-purity APT as raw material, and prepares high-purity WO by adopting a sectional calcination process after gas breaking pretreatment 3 And then high-purity tungsten powder is prepared by high-temperature hydrogen reduction. By adopting the preparation method of the high-purity tungsten powder, the high-purity tungsten powder with complete crystal grain development, low activity and low C, O, N, H content can be prepared, the requirement of the high-purity sputtering target material for the semiconductor can be better met, and the preparation method has very wide application market prospect in the field of semiconductor integrated circuits or solar photovoltaic sputtering coating.

Description

Preparation method of high-purity tungsten powder with controlled content of non-metallic elements
Technical Field
The invention belongs to the field of powder metallurgy, and particularly relates to a preparation method of high-purity tungsten powder with controlled content of non-metallic elements.
Background
The target material is a key core material in the fields of semiconductors, display panels, heterojunction photovoltaics and the like, and the process cannot be replaced. According to the calculation, the global target market scale in 2019 is about 160 hundred million dollars, and the total domestic demand accounts for over 30 percent. The supply of local manufacturers accounts for about 30% of the domestic market, medium and low-end products are mainly used, high-end targets are mainly imported from America, Japan and Korean, and the total target income of domestic head enterprises is in the range of 30-40 million yuan, which accounts for about 10% of the total domestic demand. Policies such as national 863 plan, 02 special project, imported tariff, material strong national strategy and the like are supported vigorously, and domestic substitution is imperative and has huge space. In 2020, the global flat panel display target market scale is about $ 52 million, and the composite velocity is increased by about 8%. The domestic market scale is about 165.9 million yuan, the composite speed is increased by about 20 percent, and the global ratio is about 47 percent. The future development trend is as follows: 5N-grade high purity, large size, high sputtering rate and precise control of crystal grain orientation. In 2020, the global market scale of the semiconductor target reaches $ 15.67 hundred million, the market scale of the semiconductor target in China is about 29.86 hundred million yuan, and 90 percent of the market share of the chip target is monopolized by manufacturers in the United states. The chip is the most top application field of the target material, and is mainly used in two links of 'wafer manufacturing' and 'chip packaging', wherein the dielectric layer, the conductor layer and the protective layer are all used for sputtering and coating the target material with the purity of more than 5N grade, and advanced processing requires metal with higher purity. The chip target has the characteristics of multiple varieties, high threshold and customized research and development, mainly uses copper, tantalum, aluminum and titanium to construct a circuit interconnection conductor in an integrated circuit. With the rise of 5G and global wafer fabrication capacity shift, large fund and policy support, the domestic chip fabrication market is developing rapidly. The chip has the most severe technical requirements on the sputtering target. In recent years, with the rapid development of information technology, the integration degree of semiconductor chips is higher and higher, so that the sizes of the semiconductor chips are continuously reduced, and new technical challenges are provided for high-purity sputtering targets.
The target material industry chain is basically distributed in a pyramid shape. The industrial chain mainly comprises four links of metal purification, target material manufacturing, sputtering coating and terminal application. The sputtering coating is the link with the highest technical requirement in the whole industrial chain. The quality of the sputtered film has a significant impact on the quality of downstream products. Sputtering is one of the main techniques for preparing thin film materials, and is characterized in that ions generated by an ion source are accelerated and gathered in vacuum to form ion beam flow with high speed energy, the ion beam flows bombard the surface of a solid, kinetic energy exchange is carried out between the ions and atoms on the surface of the solid, the atoms on the surface of the solid leave the solid and are deposited on the surface of a substrate, and the bombarded solid is a raw material for preparing a thin film deposited by a sputtering method and is called as a sputtering target material. The purity of the sputtering film is closely related to that of the sputtering target, in order to meet the requirements of the semiconductor technology with higher precision and finer micron, the purity of the required sputtering target is continuously increased and generally reaches more than 99.999 percent (5N) purity, and advanced processing requires metal with higher purity. When the sputtering target is bombarded by high-speed ion beams, the gas existing in the gap inside the sputtering target is suddenly released, so that large-size sputtering target particles are splashed, and the quality of a sputtering film is reduced and even the product is scrapped due to the appearance of the particles.
Tungsten is a metal with the highest known melting point in the world (3410 ℃), and is a very important strategic rare metal because the tungsten has the characteristics of high melting point, high hardness, stable chemical property, radiation resistance and the like, is widely applied to the fields of high-end tools, electronic information, military and national defense, aerospace, nuclear engineering and the like. Tungsten is a refractory nonferrous metal and an important strategic resource, and is widely applied due to its excellent properties such as high melting point, high hardness, strong ductility, wear resistance, corrosion resistance and the like. Tungsten has the advantages of good conductivity, good thermal stability and the like, and is widely applied to the field of sputtering coating of semiconductor integrated circuits, solar photovoltaics and the like. Tungsten has very strong physical properties, is a metal with the highest melting point in all non-alloys, has the highest corrosion resistance and tensile strength, and is known as an industrial tooth. Like all mining industry chains, the most upstream of the tungsten industry chain is tungsten ore, the intermediate products are Ammonium Paratungstate (APT) and tungsten oxide, and the downstream deep processing products are tungsten wires, tungsten powder, tungsten carbide and hard alloy. High-purity tungsten (5N) is widely used as a gate electrode material, a wiring material and a shielding metal material of a semiconductor lsi circuit because of its high electromigration resistance, high temperature stability and very high electron emission coefficient. The high-purity metal tungsten target is one of basic materials for manufacturing integrated circuits, and the market prospect of the high-purity metal tungsten target is closely related to the development of the integrated circuits; if the purity of the tungsten target is not high, the operation reliability of the large-scale integrated circuit is reduced, and even a current leakage phenomenon is generated. The high-purity tungsten is adopted, so that the influence of harmful impurities can be reduced and even eliminated, and the performance of a terminal product is improved.
The high-purity sputtering tungsten target for the semiconductor is a key material for preparing a tungsten film material through sputtering deposition, and the performance of the tungsten film depends on the purity, the density, the tissue uniformity and the like of the high-purity tungsten target. The preparation method of high-purity tungsten can be divided into a powder metallurgy method, a smelting method and a chemical vapor deposition method. The powder metallurgy method is that tungsten powder is heated to a certain temperature below the melting point of the tungsten powder after being formed, and the densification process is completed through material migration, so that tungsten blanks or certain tungsten products with simple shapes can be finally obtained. The smelting method is a process of heating a tungsten raw material to a temperature above the melting point of the tungsten raw material to form a liquid phase, removing impurities, and then cooling and solidifying to realize densification. The smelting method has great advantages in the aspect of purifying refractory metals due to the characteristics of high temperature, no pollution, good purification effect and the like; but the purity requirement of raw materials is high, the cost is high, and the process is time-consuming. Chemical vapor deposition refers to the deposition of tungsten compound gas (usually WF) 6 ) Is a tungsten source and is heated at a certain temperature by H 2 Reducing, depositing the tungsten produced on a specific substrateAnd (3) removing the substrate material after the deposition is finished to obtain a compact tungsten blank (or product). Among them, the powder metallurgy method is a main way of preparing a high purity tungsten target, and thus the performance of the high purity tungsten target greatly depends on the performance of the raw material tungsten powder. The total impurity element content of the high-purity tungsten powder is required to be controlled to be (1-10) x 10 -6 Meanwhile, the content of some special impurity elements, such as alkali metal elements, heavy metal radioactive elements, gas elements and the like, is more strictly required. The content of non-metal elements in the target material is crucial to the performance of the sputtered film. C. O, N, which may impair the stability of the film and cause an increase in the film resistance; therefore, the method is extremely important for controlling the content of the non-metallic element impurities in the raw material high-purity tungsten powder. Because the preparation process of the high-purity tungsten is complicated, and meanwhile, the effects of various purification methods on removing different impurities are greatly different; in the aspect of the preparation process of high-purity tungsten in China, the simple vacuum degassing treatment is still adopted to remove interstitial impurities, and the product purity is limited to a certain extent. Therefore, how to successfully prepare the high-purity tungsten by organically combining various processes becomes a research hotspot and difficulty. How to improve the purification process to prepare high-purity tungsten and related products with more excellent performance and realize the industrialization thereof is an important development direction in the future.
The invention provides a method for controlling the content of non-metal elements (C, H, O, N) in high-purity tungsten powder in order to effectively reduce the content of the non-metal elements (C, H, O, N) in the high-purity tungsten powder, so that the high-purity tungsten powder meeting the requirements for higher performance is prepared.
Disclosure of Invention
The invention provides a preparation method of high-purity tungsten powder capable of controlling the content of non-metal elements in order to effectively reduce the content of the non-metal elements (C, H, O, N) in the high-purity tungsten powder, so that the high-purity tungsten powder meeting the requirements and having higher performance is prepared.
In one aspect of the invention, the invention provides a method for preparing high-purity WO (tungsten trioxide) by using high-purity APT (5N and above) as a raw material and adopting a sectional calcination process after gas breaking pretreatment 3 (5N and above) and then high-purity tungsten powder (5N and above) was prepared by high-temperature hydrogen reduction.
In one aspect of the present invention, the present invention provides a method for preparing high purity tungsten powder by controlling the content of non-metallic elements, comprising the steps of:
(1) high-purity APT is taken as a raw material, and is pretreated by air flow classification;
(2) calcining the pretreated APT, and sieving to obtain high-purity WO 3 ；
(3) To prepare high-purity WO 3 Introducing high-purity hydrogen into the raw materials to carry out reduction treatment, and sieving to obtain the high-purity tungsten powder.
(4) And introducing high-purity argon into the high-purity tungsten powder for heat preservation treatment to obtain the high-purity tungsten powder.
In addition, the preparation method of the high-purity silicon tungsten powder can also have the following additional technical characteristics:
further, the high-purity APT in the step (1) is 5N or more, namely the purity is more than 99.999%;
further, the grading frequency in the step (1) is 6-12 HZ, and high-purity APT with concentrated particle size distribution and more cracks is obtained after air flow grading pretreatment;
further, the high purity WO described in the step (2) 3 5N and above, namely the purity is above 99.999%;
further, the calcining treatment in the step (2) comprises calcining for 0.5 to 2 hours at 480 to 540 ℃, and then calcining for 1 to 3 hours at 800 to 900 ℃;
further, the high-purity hydrogen in the step (3), namely the purity is more than 99.999%;
further, in the step (3), the reduction treatment temperature is 950-1050 ℃, and the reduction treatment time is 4-8 hours;
further, the high-purity argon in the step (4), namely the purity is more than 99.999%;
further, in the step (4), the heat preservation treatment temperature is 700-850 ℃, and the heat preservation treatment time is 1-3 hours;
further, the high-purity tungsten powder in the step (4) is 5N or more, namely the purity is more than 99.999%;
further, the granularity of the high-purity tungsten powder in the step (4) is 1.8-2.7 mu m;
furthermore, the content of non-metal elements in the high-purity tungsten powder in the step (4) is less than or equal to 30ppm of C, less than or equal to 30ppm of N, less than or equal to 30ppm of H and less than or equal to 800ppm of O.
Further, in one aspect of the invention, the invention also provides high-purity tungsten powder prepared by the method.
Further, in one aspect of the invention, the invention also provides application of high-purity tungsten powder in a high-purity sputtering target material for a semiconductor, wherein the high-purity tungsten powder is prepared by the method.
Further, in one aspect of the invention, the invention also provides application of a high-purity sputtering target material prepared from the high-purity tungsten powder in the field of semiconductor integrated circuits or solar photovoltaic sputtering coating, wherein the high-purity tungsten powder is prepared by the method. The high-purity tungsten product comprises a target material, a foil, a sheet, a wire, a line, a rod, powder, a monocrystal and the like, and is mainly applied to the fields of integrated circuit industry (used as an electrode material, a wiring material, a shielding material and the like) and solar photovoltaic sputtering coating.
The invention has the beneficial effects that:
1. adopt the hierarchical preliminary treatment of air current, can effectively get rid of superfine particle and thick granule in the APT (superfine and thick granule are all compacter, are unfavorable for the discharge of calcination in-process steam and ammonia), simultaneously because the APT granule is more fragile, can realize crushing effect on the classification wheel at the large granule striking, promote APT granule crackle to produce.
2. The sectional calcining process can effectively reduce the C, N content in the tungsten oxide, wherein C is less than or equal to 30ppm, and N is less than or equal to 30 ppm. Wherein, the calcination at the low temperature of 480-540 ℃ can lead the high-purity APT to generate a large amount of cracks in the decomposition process, thereby promoting the water and ammonia gas generated by the APT decomposition to be discharged in time, and further reducing the N content in the tungsten oxide. Calcination at 800-900 deg.c can ensure complete APT decomposition without residual ammonia, and the high temperature can complete the crystallization of tungsten oxide and reduce the active adsorption activity of tungsten oxide particle, so as to reduce C, N content in tungsten oxide.
3. High-purity tungsten powder with complete crystal grain development, low activity and low C, O, N, H content can be prepared by high-temperature hydrogen reduction.
4. The content of H can be effectively reduced by introducing high-purity argon under the heating condition and preserving the heat, and the content of C, O, N can be further reduced. The powder can be activated under the heating condition to promote the adsorption of the powder on gas; meanwhile, high-concentration high-purity argon is introduced to replace C, O, N, H element with low content adsorbed on the powder.
Drawings
In order to facilitate understanding for those skilled in the art, the invention is further described below with reference to the accompanying drawings.
FIG. 1 is a process flow diagram of the preparation method of high purity tungsten powder of the present invention.
Detailed Description
The present invention will be further described below for better understanding the objects, technical solutions and advantages thereof, without limiting the scope of the present invention to the following examples, which are only intended to illustrate the present invention in detail and are not intended to limit the scope of the present invention in any way. The instruments and devices referred to in the following examples are conventional instruments and devices unless otherwise specified; the raw materials are all conventional commercial industrial raw materials if not specifically indicated; the processing and manufacturing methods are conventional methods unless otherwise specified. It should be understood that the description is intended to be exemplary only, and is not intended to limit the scope of the present invention. Moreover, in the following description, descriptions of well-known structures and techniques are omitted so as to not unnecessarily obscure the concepts of the present invention.
The invention provides a preparation method of high-purity tungsten powder capable of controlling the content of non-metal elements in order to effectively reduce the content of the non-metal elements (C, H, O, N) in the high-purity tungsten powder, so that the high-purity tungsten powder meeting the requirements and having higher performance is prepared.
In one aspect of the invention, the invention provides a method for preparing high-purity WO (tungsten trioxide) by using high-purity APT (5N and above) as a raw material and adopting a sectional calcination process after gas breaking pretreatment 3 (5N and above) and then high-purity tungsten powder (5N and above) was prepared by high-temperature hydrogen reduction.
In one aspect of the present invention, the present invention provides a method for preparing high purity tungsten powder with controlled content of non-metallic elements, comprising the steps of:
(1) high-purity APT is used as a raw material, and is pretreated by air flow classification;
(2) calcining the pretreated APT, and sieving to obtain high-purity WO 3 ；
(3) To prepare high-purity WO 3 Introducing high-purity hydrogen into the raw materials to carry out reduction treatment, and sieving to obtain high-purity tungsten powder;
(4) and introducing high-purity argon into the high-purity tungsten powder for heat preservation treatment to obtain the high-purity tungsten powder.
Further, in the examples of the present invention, the high purity APT in step (1) is 5N or more, that is, the purity is 99.999% or more. High-purity Ammonium Paratungstate (APT) is the most important high-purity tungsten raw material and is generally prepared by tungsten ore leaching-extraction and transformation-deep purification-evaporative crystallization. The high-end tungsten product has strict requirements on impurity removal, the purity requirement on the raw material ammonium paratungstate is improved, and the impurity content needs to be strictly controlled in the process of purifying the tungsten raw material, so that high-purity raw materials are provided for producing high-performance and high-quality tungsten products by subsequent processes. The existing methods for preparing high-purity APT by controlling the content of impurities in industrial production comprise a redissolution method, an ion exchange method, an ammonium metatungstate method, an electrolytic method, a recrystallization method and the like. However, because of the different chemical properties of impurity elements, it is difficult to remove all impurities by one method, so that the preparation of high-purity APT usually requires further purification by means of secondary ion exchange, activated carbon adsorption and the like. However, the high purity APT of the present invention is not particularly limited, and commercially available high purity tungsten powder known to those skilled in the art may be used.
Further, in the embodiment of the invention, the classification frequency in the step (1) is 6-12 Hz, and the high-purity APT with concentrated particle size distribution and more cracks is obtained after air flow classification pretreatment.
Further, in the embodiment of the present invention, by using the airflow classification pretreatment, the ultrafine particles and coarse particles in the APT can be effectively removed (the ultrafine particles and the coarse particles are dense and are not beneficial to discharge of water vapor and ammonia gas during the calcination process), and meanwhile, due to the brittleness of the APT particles, the large particles can be crushed when impacting on the classification wheel, so as to promote the generation of cracks in the APT particles. Gas stream classification is a particle classification operation that utilizes the difference in settling velocity of particles in a gas stream. The airflow carrying the powder particles is subjected to methods of reducing the flow speed, changing the flow direction and the like to settle coarse particles and carry away fine particles, so that coarse and fine powder particles are separated. The equipment for air classification is called a separator, also called a coarse powder separator. Closed cycles are usually formed in combination with dry grinding machines. The airflow containing powder from the grinding machine is fed from the air inlet pipe at a certain speed, the coarse powder is collided back by the reflecting cone and settled, because the cross-sectional area of the flow passage between the inner cone and the outer cone is gradually enlarged, the airflow speed in the flow passage is reduced to a certain speed, the secondary coarse powder is also settled, the airflow enters the inner cone through the shutter, centrifugal settlement is generated due to the rotation movement, a part of powder particles are separated, the finest powder is carried out along with the airflow, the powder particles are recovered by a filtering method and are used as ground finished products, and the coarse particles separated in the separator are collected and returned to the grinding machine. However, the present invention is not limited to any particular gas flow classifying apparatus, and any commercially available or self-made gas flow classifying apparatus known to those skilled in the art may be used.
Further, in the examples of the present invention, the high purity WO described in the step (2) 3 5N or more, that is, the purity is 99.999% or more.
Further, in the embodiment of the invention, the calcination treatment in the step (2) is firstly calcination at 480-540 ℃ for 0.5-2 h, and then calcination at 800-900 ℃ for 1-3 h. The inventor researches and finds that the high-purity tungsten powder provided by the invention can be prepared more easily within the reasonable temperature and time range. If the sintering temperature is too low, the sintering effect is poor, and the situation of insufficient and incomplete sintering is easy to occur; if the sintering temperature is too high, solid-phase agglomeration is easily formed seriously, and the uniformity of the powder is reduced. In addition, the excessively high sintering temperature has higher requirements on equipment and higher cost, and is not beneficial to subsequent large-scale industrial production. The sintering time is too short, and a good full sintering effect cannot be realized; and if the sintering time is too long, energy is wasted, the cost is increased, and the subsequent large-scale industrial production is not facilitated. Therefore, the sintering temperature and the sintering time within the above ranges of the present invention can ensure the best calcination treatment effect.
Further, in the embodiment of the invention, the content of C, N in tungsten oxide can be effectively reduced by the sectional calcination process, wherein C is less than or equal to 30ppm, and N is less than or equal to 30 ppm. Wherein, the calcination at the low temperature of 480-540 ℃ can lead the high-purity APT to generate a large amount of cracks in the decomposition process, thereby promoting the water and ammonia gas generated by the APT decomposition to be discharged in time, and further reducing the N content in the tungsten oxide. Calcination at 800-900 deg.c can ensure complete APT decomposition without residual ammonia, and the high temperature can complete the crystallization of tungsten oxide and reduce the active adsorption activity of tungsten oxide particle, so as to reduce C, N content in tungsten oxide.
Further, in the embodiment of the present invention, the purity of the high-purity hydrogen in the step (3), that is, the purity is 99.999% or more. The hydrogen purification method mainly comprises a low-temperature adsorption method, a low-temperature liquefaction method and a metal hydride hydrogen purification method; further, there are a palladium membrane diffusion method, a hollow fiber membrane diffusion method, a pressure swing adsorption method, and the like. Hydrogen is a major industrial raw material and one of the major secondary energy sources in the future. Hydrogen is a main industrial raw material, is also the most important industrial gas and special gas, and has wide application in the fields of petrochemical industry, electronic industry, metallurgical industry, food processing, float glass, fine organic synthesis, aerospace and the like. Meanwhile, hydrogen is an ideal secondary energy source. In general, hydrogen is very easily combined with oxygen. This property makes it a natural reducing agent for use in production to prevent oxidation. In the high temperature processing of glass manufacture and the manufacture of electronic microchips, hydrogen is added to a nitrogen atmosphere to remove residual oxygen. In the petrochemical industry, hydrogenation is required to refine crude oil by desulfurization and hydrocracking. Another important use of hydrogen is in the hydrogenation of fats in margarines, edible oils, shampoos, lubricants, household cleaners and other products. The aerospace industry uses liquid hydrogen as a fuel due to the high fuel properties of hydrogen. However, the present invention is not limited to any particular method, and any commercially available high-purity hydrogen gas or any self-made high-purity hydrogen gas having the above purity requirement, which is well known to those skilled in the art, may be used.
Further, in the embodiment of the invention, the reduction treatment temperature in the step (3) is 950-1050 ℃, and the reduction treatment time is 4-8 h; high-purity tungsten powder with complete crystal grain development, low activity and low C, O, N, H content can be prepared by high-temperature hydrogen reduction. The inventor researches and finds that the high-purity tungsten powder provided by the invention can be prepared more easily within the reasonable temperature and time range. If the reduction treatment temperature is too low, the reduction effect is poor, and the situation of insufficient and incomplete reduction is easy to occur; if the reduction temperature is too high, the situation of over reduction is easy to occur; in addition, the excessively high reduction temperature has higher requirements on equipment and higher cost, and is not beneficial to subsequent large-scale industrial production. The reduction time is too short, so that a good full and complete reduction effect cannot be realized; and if the reduction time is too long, energy is wasted, the cost is increased, and the subsequent large-scale industrial production is not facilitated. Thus, the optimum reduction effect can be ensured by using the reduction temperature and the reduction time within the above-described ranges of the present invention.
Further, in the embodiment of the present invention, the purity of the argon gas in the step (4) is high, that is, the purity is 99.999% or more. Argon is a colorless, tasteless, odorless and nontoxic inert gas, cannot be combusted and support combustion, does not react with other substances at normal temperature, and has very inert chemical properties and good stability. Argon, which is present in air at very low levels, only 0.93%, is typically isolated as a by-product from air separation oxygen generation. High-purity argon is an essential purifying and shielding gas in the preparation process of monocrystalline silicon and polycrystalline silicon, the required purity is usually more than 99.999 percent, and the production cost is higher. High purity argon is a colorless, odorless, nontoxic gas. The chemical property is very inactive, and no compound is formed. And (3) extracting argon by adopting air separation, namely rectifying liquefied air to obtain crude argon. The crude argon is pumped out and further purified to obtain the high-purity argon. High purity argon is used in the semiconductor industry as a shielding gas for the production of high purity silicon and germanium crystals; can be used as inert gas for cleaning, shielding and pressurizing the system; the method is applied to the processes of chemical vapor deposition, sputtering, annealing and the like. High purity argon may also be used as a chromatographic carrier gas. Argon is widely used to fill arc lamps, fluorescent lamps and electron tubes; welding shielding gas; as shielding gas in the production of titanium, cobalt and other active metals; in ferrous metallurgy for converting special steels. However, the present invention does not have any more specific limitation on the high purity argon, and commercially available high purity argon known to those skilled in the art or self-made high purity argon meeting the above purity requirements may be used.
Further, in the embodiment of the invention, the heat preservation treatment temperature in the step (4) is 700-850 ℃, and the heat preservation treatment time is 1-3 h; the high-purity argon is introduced under the heat preservation and heating conditions, so that the H content can be effectively reduced, and the C, O, N content is further reduced. The powder can be activated under the heating condition to promote the adsorption of the powder on gas; meanwhile, high-concentration high-purity argon is introduced to replace C, O, N, H element with low content adsorbed on the powder. The inventor researches and finds that the high-purity tungsten powder can be prepared more easily within the reasonable temperature and time range. If the temperature of the heat preservation treatment is too low, the effect is not ideal; and the heat preservation treatment temperature is too high, so that the requirement on equipment is higher, the cost is higher, and the subsequent large-scale industrial production is not facilitated. The heat preservation treatment time is too short, so that a good heat preservation treatment effect cannot be realized; and the heat preservation treatment time is too long, so that energy is wasted, the cost is increased, and the subsequent large-scale industrial production is not facilitated. Therefore, the optimal heat preservation treatment effect can be ensured by adopting the heat preservation treatment temperature and the heat preservation treatment time within the range.
Further, in the embodiment of the present invention, the high purity tungsten powder in the step (4) is 5N or more, that is, the purity is 99.999% or more;
further, in the embodiment of the invention, the particle size of the high-purity tungsten powder in the step (4) is 1.8-2.7 μm;
further, in the embodiment of the invention, the content of non-metal elements in the high-purity tungsten powder in the step (4) is less than or equal to 30ppm of C, less than or equal to 30ppm of N, less than or equal to 30ppm of H and less than or equal to 800ppm of O;
further, in one aspect of the invention, the invention also provides high-purity tungsten powder prepared by the method. The product processed by the high-purity tungsten powder has the advantages of greatly reduced impurities, stable performance, uniform texture, smooth appearance, long service life and the like, fully shows the advantages and the characteristics of tungsten element, and is widely applied to the industries of high-end light sources such as electrodes for ultrahigh-pressure discharge lamps, semiconductor-grade magnetron sputtering targets and the like, electronics, semiconductors and the like.
Further, in one aspect of the invention, the invention also provides application of high-purity tungsten powder in a high-purity sputtering target material for a semiconductor, wherein the high-purity tungsten powder is prepared by the method. The high-purity tungsten product comprises a target material, a foil, a sheet, a wire, a line, a rod, powder, a monocrystal and the like, and is mainly applied to the fields of integrated circuit industry (used as an electrode material, a wiring material, a shielding material and the like) and solar photovoltaic sputtering coating.
Further, in one aspect of the invention, the invention also provides application of a high-purity sputtering target material prepared from the high-purity tungsten powder in the field of semiconductor integrated circuits or solar photovoltaic sputtering coating, wherein the high-purity tungsten powder is prepared by the method. The chip is the most top application field of the target material, and is mainly used in two links of 'wafer manufacturing' and 'chip packaging', wherein the dielectric layer, the conductor layer and the protective layer are all used for sputtering and coating the target material with the purity of more than 5N grade, and advanced processing requires metal with higher purity. The high-purity tungsten powder prepared by the method can be used for preparing high-purity sputtering target materials with higher purity and more practical application in the field of semiconductors. In recent years, with the rise of 5G and global wafer fabrication yield shift, the domestic chip fabrication market has been accelerated with support of large funds and policies. The chip has the most severe technical requirements for sputtering the target material. With the rapid development of information technology, the integration level of semiconductor chips is higher and higher, so that the size of the semiconductor chips is continuously reduced, and a new technical challenge is provided for high-purity sputtering targets. The high-purity tungsten powder prepared by the method can better meet the application of high-purity sputtering target materials in the field of semiconductor integrated circuits or solar photovoltaic sputtering coating, and has very wide prospect.
The invention will now be described with reference to specific examples, which are intended to be illustrative only and not to be limiting in any way.
Example 1:
1. carrying out air flow grading pretreatment by taking high-purity APT as a raw material, wherein the frequency of a grading wheel is 6 HZ;
2. calcining at 480 ℃ for 2h, calcining at 850 ℃ for 1.5h, and sieving to obtain the high-purity WO 3 ；
3. To obtain high-purity WO 3 Introducing high-purity hydrogen to reduce the tungsten powder for 6 hours at 950 ℃, and sieving the tungsten powder to obtain high-purity tungsten powder;
4. introducing high-purity argon into the high-purity tungsten powder at 700 ℃ and preserving the heat for 3 hours;
5. the granularity of the high-purity tungsten powder is 1.8 mu m, wherein the content of non-metallic elements C: 30ppm, N: 30ppm, H: 28ppm, O: 700 ppm.
Example 2:
1. carrying out air flow grading pretreatment by taking high-purity APT as a raw material, wherein the frequency of a grading wheel is 6 HZ;
2. calcining at 500 deg.C for 1.5h, calcining at 850 deg.C for 1.5h, and sieving to obtain high purity WO 3 ；
3. To prepare high-purity WO 3 Introducing high-purity hydrogen to reduce the tungsten powder for 6 hours at 950 ℃, and sieving the tungsten powder to obtain high-purity tungsten powder;
4. introducing high-purity argon into the high-purity tungsten powder at 700 ℃ and preserving the heat for 3 hours;
5. the granularity of the high-purity tungsten powder is 1.8 mu m, wherein the content of non-metallic elements C: 23ppm, N: 20ppm, H: 28ppm, O: 700 ppm.
Example 3:
1. carrying out air flow grading pretreatment by taking high-purity APT as a raw material, wherein the frequency of a grading wheel is 8 HZ;
2. calcining at 540 deg.C for 0.8 hr, calcining at 850 deg.C for 1.5 hr, and sieving to obtain high purity WO 3 ；
2. To prepare high-purity WO 3 Introducing high-purity hydrogen to reduce the temperature of 950 ℃ for the raw materialSieving for 6h to obtain high-purity tungsten powder;
3. introducing high-purity argon into the high-purity tungsten powder at 700 ℃ and preserving the heat for 3 hours;
4. the granularity of the high-purity tungsten powder is 1.8 mu m, wherein the content of non-metallic elements C: 26ppm, N: 25ppm, H: 28ppm, O: 700 ppm.
Example 4:
1. carrying out air flow grading pretreatment by taking high-purity APT as a raw material, wherein the frequency of a grading wheel is 10 HZ;
2. calcining at 500 deg.C for 1.5h, calcining at 900 deg.C for 1.5h, and sieving to obtain high purity WO 3 ；
3. To prepare high-purity WO 3 Introducing high-purity hydrogen to reduce the tungsten powder for 6 hours at 950 ℃, and sieving the tungsten powder to obtain high-purity tungsten powder;
4. introducing high-purity argon into the high-purity tungsten powder at 700 ℃ and preserving the heat for 3 hours;
5. the granularity of the high-purity tungsten powder is 1.85 mu m, wherein the content of non-metallic elements C: 20ppm, N: 21ppm, H: 28ppm, O: 650 ppm.
Example 5:
1. carrying out air flow grading pretreatment by taking high-purity APT as a raw material, wherein the frequency of a grading wheel is 8 HZ;
2. calcining at 500 deg.C for 1.5h, calcining at 800 deg.C for 1.5h, and sieving to obtain high purity WO 3 ；
3. To prepare high-purity WO 3 Introducing high-purity hydrogen to reduce the tungsten powder for 6 hours at 950 ℃, and sieving the tungsten powder to obtain high-purity tungsten powder;
4. introducing high-purity argon into the high-purity tungsten powder at 700 ℃ and preserving the heat for 3 hours;
5. the granularity of the high-purity tungsten powder is 1.78 mu m, wherein the content of non-metallic elements C: 26ppm, N: 28ppm, H: 28ppm, O: 750 ppm.
Example 6:
1. taking high-purity APT as a raw material, carrying out gas breaking pretreatment, and then carrying out gas flow grading pretreatment, wherein the frequency of a grading wheel is 10 HZ;
2. calcining at 500 deg.C for 1.5 hr, calcining at 900 deg.C for 2.0 hr, and sieving to obtain high-purity WO 3 ；
3. To prepare high-purity WO 3 As starting material, in 9Introducing high-purity hydrogen to reduce for 6h at 50 ℃, and sieving to obtain high-purity tungsten powder;
4. introducing high-purity argon into the high-purity tungsten powder at 700 ℃ and preserving the heat for 3 hours;
5. the granularity of the high-purity tungsten powder is 1.9 mu m, wherein the content of non-metallic elements C: 18ppm, N: 17ppm, H: 26ppm, O: 610 ppm.
Example 7:
1. carrying out air flow grading pretreatment by taking high-purity APT as a raw material, wherein the frequency of a grading wheel is 8 HZ;
2. calcining at 500 deg.C for 1.5 hr, calcining at 900 deg.C for 1.0 hr, and sieving to obtain high-purity WO 3 ；
3. To prepare high-purity WO 3 Introducing high-purity hydrogen to reduce the tungsten powder for 6 hours at 950 ℃, and sieving the tungsten powder to obtain high-purity tungsten powder;
4. introducing high-purity argon into the high-purity tungsten powder at 700 ℃ and preserving the heat for 3 hours;
5. the granularity of the high-purity tungsten powder is 1.8 mu m, wherein the content of non-metallic elements C: 22ppm, N: 23ppm, H: 28ppm, O: 700 ppm.
Example 8:
1. carrying out air flow grading pretreatment by taking high-purity APT as a raw material, wherein the frequency of a grading wheel is 12 HZ;
2. calcining at 500 deg.C for 1.5h, calcining at 900 deg.C for 2h, and sieving to obtain high purity WO 3 ；
3. To prepare high-purity WO 3 Introducing high-purity hydrogen to reduce the tungsten powder for 5 hours at 1000 ℃, and sieving the tungsten powder to obtain high-purity tungsten powder;
4. introducing high-purity argon into the high-purity tungsten powder at 700 ℃ and preserving the heat for 3 hours;
5. the granularity of the high-purity tungsten powder is 2.3 mu m, wherein the content of non-metallic elements C: 16ppm, N: 15ppm, H: 24ppm, O: 450 ppm.
Example 9:
1. carrying out air flow grading pretreatment by taking high-purity APT as a raw material, wherein the frequency of a grading wheel is 12 HZ;
2. calcining at 500 deg.C for 1.5h, calcining at 900 deg.C for 2h, and sieving to obtain high purity WO 3 ；
3. To prepare high-purity WO 3 As a raw material, in 1Introducing high-purity hydrogen to reduce for 4h at the temperature of 050 ℃, and sieving to obtain high-purity tungsten powder;
4. introducing high-purity argon into the high-purity tungsten powder at 700 ℃ and preserving the heat for 3 hours;
5. the granularity of the high-purity tungsten powder is 2.7 mu m, wherein the content of non-metallic elements C: 14ppm, N: 13ppm, H: 21ppm, O: 400 ppm.
Example 10:
1. carrying out air flow grading pretreatment by taking high-purity APT as a raw material, wherein the frequency of a grading wheel is 8 HZ;
2. calcining at 500 deg.C for 1.5h, calcining at 900 deg.C for 2h, and sieving to obtain high purity WO 3 ；
3. To prepare high-purity WO 3 Introducing high-purity hydrogen into the raw materials at 1050 ℃ to reduce the raw materials for 4 hours, and sieving the raw materials to obtain high-purity tungsten powder;
4. introducing high-purity argon into the high-purity tungsten powder at 800 ℃ and preserving the heat for 3 hours;
5. the granularity of the high-purity tungsten powder is 2.7 mu m, wherein the content of non-metallic elements C: 12ppm, N: 11ppm, H: 19ppm, O: 380 ppm.
Example 11:
1. carrying out air flow grading pretreatment by taking high-purity APT as a raw material, wherein the frequency of a grading wheel is 8 HZ;
2. calcining at 500 deg.C for 1.5h, calcining at 900 deg.C for 2h, and sieving to obtain high purity WO 3 ；
3. To prepare high-purity WO 3 Introducing high-purity hydrogen to reduce the raw materials for 4 hours at 1050 ℃, and sieving to obtain high-purity tungsten powder;
4. introducing high-purity argon into the high-purity tungsten powder at 850 ℃ and preserving the heat for 3 hours;
5. the granularity of the high-purity tungsten powder is 2.7 mu m, wherein the content of non-metallic elements C: 11ppm, N: 10ppm, H: 17ppm, O: 370 ppm.
Example 12:
1. carrying out air flow grading pretreatment by taking high-purity APT as a raw material, wherein the frequency of a grading wheel is 8 HZ;
2. calcining at 500 deg.C for 1.5h, calcining at 900 deg.C for 2h, and sieving to obtain high purity WO 3 ；
3. To prepare high-purity WO 3 As a raw material, inReducing for 4h at 1050 ℃ by introducing high-purity hydrogen, and sieving to obtain high-purity tungsten powder;
4. introducing high-purity argon into the high-purity tungsten powder at 850 ℃ and keeping the temperature for 5 hours;
5. the granularity of the high-purity tungsten powder is 2.7 mu m, wherein the content of non-metallic elements C: 10ppm, N: 10ppm, H: 15ppm, O: 360 ppm.
Example 13:
1. carrying out air flow grading pretreatment by taking high-purity APT as a raw material, wherein the frequency of a grading wheel is 10 HZ;
2. calcining at 500 deg.C for 1.5h, calcining at 900 deg.C for 2h, and sieving to obtain high purity WO 3 ；
3. To prepare high-purity WO 3 Introducing high-purity hydrogen to reduce the raw materials for 4 hours at 1050 ℃, and sieving to obtain high-purity tungsten powder;
4. introducing high-purity argon into the high-purity tungsten powder at 850 ℃ and keeping the temperature for 7 hours;
5. the granularity of the high-purity tungsten powder is 2.7 mu m, wherein the content of non-metallic elements C: 10ppm, N: 10ppm, H: 13ppm, O: 360 ppm.
Comparative example 1:
1. calcining high-purity APT (ammonium paratungstate) serving as a raw material at 500 ℃ for 1.5h and 900 ℃ for 2h, and sieving to obtain high-purity WO 3 ；
2. To prepare high-purity WO 3 Introducing high-purity hydrogen into the raw materials at 1050 ℃ to reduce the raw materials for 4 hours, and sieving the raw materials to obtain high-purity tungsten powder;
3. introducing high-purity argon into the high-purity tungsten powder at 850 ℃ and keeping the temperature for 7 hours;
4. the granularity of the high-purity tungsten powder is 2.7 mu m, wherein the content of non-metallic elements C: 16ppm, N: 16ppm, H: 13ppm, O: 360 ppm.
Comparative example 2:
1. carrying out air flow grading pretreatment by taking high-purity APT as a raw material, wherein the frequency of a grading wheel is 10 HZ;
2. calcining at 900 ℃ for 3.5h, and sieving to obtain high-purity WO 3 ；
3. To prepare high-purity WO 3 Introducing high-purity hydrogen to reduce the raw materials for 4 hours at 1050 ℃, and sieving to obtain high-purity tungsten powder;
4. introducing high-purity argon into the high-purity tungsten powder at 850 ℃ and keeping the temperature for 7 hours;
5. the granularity of the high-purity tungsten powder is 2.6 mu m, wherein the content of non-metallic elements C: 20ppm, N: 15ppm, H: 15ppm, O: 400 ppm.
Comparative example 3:
1. carrying out air flow grading pretreatment by taking high-purity APT as a raw material, wherein the frequency of a grading wheel is 6 HZ;
2. calcining at 500 deg.C for 1.5h, calcining at 900 deg.C for 2h, and sieving to obtain high purity WO 3 ；
3. To prepare high-purity WO 3 Introducing high-purity hydrogen into the raw materials at 1050 ℃ to reduce the raw materials for 4 hours, and sieving the raw materials to obtain high-purity tungsten powder;
4. introducing high-purity argon into the high-purity tungsten powder at 850 ℃ and keeping the temperature for 7 hours;
5. the granularity of the high-purity tungsten powder is 2.7 mu m, wherein the content of non-metallic elements C: 14ppm, N: 14ppm, H: 13ppm, O: 360 ppm.
Comparative example 4:
1. carrying out air flow grading pretreatment by taking high-purity APT as a raw material, wherein the frequency of a grading wheel is 12 HZ;
2. calcining at 900 ℃ for 3.5h, and sieving to obtain high-purity WO 3 ；
3. To prepare high-purity WO 3 Introducing high-purity hydrogen to reduce the raw materials for 4 hours at 1050 ℃, and sieving to obtain high-purity tungsten powder;
4. introducing high-purity argon into the high-purity tungsten powder at 850 ℃ and keeping the temperature for 7 hours;
5. the granularity of the high-purity tungsten powder is 2.6 mu m, wherein the content of non-metallic elements C: 30ppm, N: 23ppm, H: 15ppm, O: 400 ppm.
Comparative example 5:
1. carrying out air flow grading pretreatment by taking high-purity APT as a raw material, wherein the frequency of a grading wheel is 12 HZ;
2. calcining at 500 deg.C for 1.5h, calcining at 900 deg.C for 2h, and sieving to obtain high purity WO 3 ；
3. To prepare high-purity WO 3 Introducing high-purity hydrogen to reduce the raw materials for 4 hours at 1050 ℃, and sieving to obtain high-purity tungsten powder;
4. introducing high-purity argon into the high-purity tungsten powder at 850 ℃ and keeping the temperature for 7 hours;
5. the granularity of the high-purity tungsten powder is 2.6 mu m, wherein the content of non-metallic elements C: 25ppm, N: 20ppm, H: 15ppm, O: 400 ppm.
Comparative example 6:
1. calcining high-purity APT (ammonium paratungstate) serving as a raw material at 900 ℃ for 3.5 hours, and sieving to obtain high-purity WO 3 ；
3. To prepare high-purity WO 3 Introducing high-purity hydrogen into the raw materials at 1050 ℃ to reduce the raw materials for 4 hours, and sieving the raw materials to obtain high-purity tungsten powder;
4. introducing high-purity argon into the high-purity tungsten powder at 850 ℃ and keeping the temperature for 7 hours;
5. the granularity of the high-purity tungsten powder is 2.6 mu m, wherein the content of non-metallic elements C: 40ppm, N: 35ppm, H: 15ppm, O: 400 ppm.
Comparative example 7:
1. carrying out air flow grading pretreatment by taking high-purity APT as a raw material, wherein the frequency of a grading wheel is 10 HZ;
2. calcining at 500 deg.C for 1.5h, calcining at 900 deg.C for 2h, and sieving to obtain high purity WO 3 ；
3. To prepare high-purity WO 3 Introducing high-purity hydrogen to reduce the raw materials for 4 hours at 1050 ℃, and sieving to obtain high-purity tungsten powder;
4. the granularity of the high-purity tungsten powder is 2.6 mu m, wherein the content of non-metallic elements C: 12ppm, N: 12ppm, H: 50ppm, O: 500 ppm.
Therefore, the high-purity tungsten powder prepared by the method has relatively lower content of the non-metallic element (C, H, O, N). Therefore, the high-purity tungsten powder prepared by the method has relatively higher purity.
The foregoing examples are merely illustrative of and explain the present invention and are not to be construed as limiting the scope of the invention. All the technologies realized based on the above-mentioned contents of the present invention are covered in the protection scope of the present invention.

Claims (10)

1. A preparation method of high-purity tungsten powder for controlling the content of non-metallic elements is characterized by comprising the following steps:
(1) high-purity APT is taken as a raw material, and is pretreated by air flow classification;
(2) calcining the pretreated APT, and sieving to obtain high-purity WO 3 ；
(3) To prepare high-purity WO 3 Introducing high-purity hydrogen into the raw materials to carry out reduction treatment, and sieving to obtain a high-purity tungsten powder primary product;
(4) and introducing high-purity argon into the high-purity tungsten powder primary product for heat preservation treatment to obtain the high-purity tungsten powder.
2. The method according to claim 1, wherein the high purity APT in step (1) is 5N or more, i.e., 99.999% or more.
3. The method according to claim 1, wherein the classification frequency in the step (1) is 6-12 Hz, and the high-purity APT with concentrated particle size distribution and more cracks is obtained after the pretreatment of gas flow classification.
4. The method according to any one of claims 1 to 3, wherein the high purity WO in step (2) 3 5N and above, namely the purity is above 99.999%; in the step (2), the calcination treatment is to calcine at 480-540 ℃ for 0.5-2 h and then calcine at 800-900 ℃ for 1-3 h.
5. The method according to any one of claims 1 to 3, wherein the high purity hydrogen gas in step (3) has a purity of 99.999% or more; in the step (3), the reduction treatment temperature is 950-1050 ℃, and the reduction treatment time is 4-8 h.
6. The method according to any one of claims 1 to 3, wherein the argon gas in step (4) is of high purity, i.e. has a purity of 99.999% or more; in the step (4), the heat preservation treatment temperature is 700-850 ℃, and the heat preservation treatment time is 1-3 h.
7. The method according to any one of claims 1 to 3, wherein the high purity tungsten powder in the step (4) is 5N or more, that is, has a purity of 99.999% or more; the granularity of the high-purity tungsten powder in the step (4) is 1.8-2.7 mu m.
8. A high purity tungsten powder produced by the method according to any one of claims 1 to 7.
9. The application of high-purity tungsten powder in high-purity sputtering target materials for semiconductors is characterized in that the high-purity tungsten powder is prepared by the method of any one of claims 1 to 7.
10. The application of the high-purity sputtering target material prepared from the high-purity tungsten powder in the field of semiconductor integrated circuits or solar photovoltaic sputtering coating is characterized in that the high-purity tungsten powder is prepared by the method of any one of claims 1 to 7.
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