Method for measuring volatile components of titanium sponge

Abstract

The invention relates to the technical field of metallurgy, in particular to a titanium sponge volatile component measuring method which comprises the following steps: S1, sample preparation: primarily splitting a taken sample to about 4 kilograms, splitting again in a sample pressing chamber to obtain two samples with the weight of 1 kilogram, putting the samples into a measuring cylinder, compacting, measuring the bulk density, averaging, pressing into an electrode on a hydraulic machine, and taking out the sample; polishing edges and corners of the electrode to be flat on a sand mill; s2, detection of components of the sponge titanium electrode: drilling chippings on the sponge titanium electrode according to required point positions, fully and uniformly mixing, and measuring component indexes; s3, measuring the weight of volatile components; s4, determination of titanium ingot and ash components; and S5, calculating the components of volatile components. According to the method for measuring the volatile components of the sponge titanium, factors influencing the generation of the volatile components in the production process can be deeply analyzed by accurately measuring the content and the components of the volatile components of the sponge titanium, so that reliable data support is provided for optimizing process parameters for producing the sponge titanium by a magnesiothermy method.

Description

Technical Field

[0001] The invention relates to the technical field of metallurgy, in particular to a method for measuring volatile matter of sponge titanium. Background Art

[0002] Titanium reserves are extremely abundant in the Earth's crust, ranking fourth after iron, aluminum, and magnesium. Thanks to its high melting point, low specific gravity, high specific strength, excellent toughness, fatigue resistance, corrosion resistance, low thermal conductivity, stable performance in high and low temperature environments, and low stress from rapid cooling and heating, titanium has been gaining prominence in high-tech fields such as aviation and aerospace since the 1950s, demonstrating its high commercial value. Since then, its application has continuously expanded, gradually extending to numerous industries such as chemicals, petroleum, electricity, desalination, construction, and daily necessities.

[0003] Because titanium is a reactive metal that readily reacts with oxygen in the air, its melting process must be conducted under vacuum. Currently, common vacuum melting methods include vacuum induction melting, vacuum arc melting, electron beam melting, plasma melting, and cold hearth melting. These methods all rely on vacuum pumps to remove gases from the system and create the required vacuum conditions.

[0004] During the vacuum melting process of titanium sponge, a large amount of volatiles are generated within the vacuum system. These volatiles, when mixed with moisture in the air and mechanical pump oil, can seriously harm the normal operation of mechanical equipment and the vacuum system. For example, in the chemical reaction H2O + Cl2 = HCl + HClO, the hydrochloric acid and hypochlorous acid produced by the reaction dissolve in large quantities in the vacuum pump oil, causing severe corrosion to components such as the vacuum pump chamber and the slide valve.

[0005] Currently, the mainstream method for industrial production of titanium sponge is the magnesium thermal process, which follows the process route of titanium tetrachloride → reduction → distillation → cooling → crushing → finished titanium sponge. However, the existing distillation process has limitations, making it difficult to completely remove volatiles from titanium sponge. Downstream customers frequently report that when vacuum melting titanium sponge to produce titanium ingots, the volatile content is high and accurate quantitative analysis of the volatile components is impossible. These issues hinder equipment operation, seriously affecting production efficiency and product quality.

[0006] Companies attach great importance to the problems that arise during the use of titanium sponge by downstream customers. There is an urgent need to measure the volatile content of titanium sponge so that data can be collected and organized in a timely manner, and refined management and control can be implemented in subsequent production to provide high-quality products that meet customer requirements. However, as of now, there is no effective test method for the volatile content in titanium sponge. Therefore, there is an urgent need to develop a method that can accurately measure the volatile content of titanium sponge to provide reliable data support for subsequent smelting process optimization and production experiments, so as to promote the high-quality development of the titanium sponge industry. Summary of the Invention

[0007] The present invention aims to provide a method for measuring the volatile content of titanium sponge to address the limitations of the existing distillation process outlined in the background art, which makes it difficult to completely remove volatiles from titanium sponge. Downstream customers frequently report that when vacuum melting titanium ingots using titanium sponge, the volatile content is high and accurate quantitative analysis of the volatile components is impossible. These issues hinder equipment operation, severely impacting production efficiency and product quality.

[0008] To achieve the above object, the present invention provides a method for measuring the volatile matter of titanium sponge, comprising the following steps:

[0009] S1. Sample preparation: The sample was initially reduced to approximately 4 kg, and then further reduced in the sample pressing chamber to obtain two 1 kg samples. The samples were placed in a graduated cylinder and vibrated to measure the bulk density. The average value was taken, and the electrodes were then pressed into electrodes using a hydraulic press, and the edges and corners of the electrodes were smoothed using a sand grinder.

[0010] S2. Detection of the composition of the titanium sponge electrode: Drill chips at the required points on the titanium sponge electrode, mix them thoroughly and measure the composition indicators, which include Fe, Si, Cl, C, N, O, Mn, Mg, H, Ni, Cr, Sn, and Al;

[0011] S3. Determination of volatile matter weight;

[0012] S4, titanium ingot, determination of ash composition;

[0013] S5. Calculation of volatile components.

[0014] This setting builds the overall process framework for the measurement of sponge titanium volatiles. In the sample preparation stage, the sample is processed to an appropriate weight through initial and secondary reduction to ensure the representativeness of the sample and the feasibility of subsequent operations; the bulk density is measured and the electrodes are pressed and polished to provide a standard sample shape for subsequent component detection and volatile determination. In the component detection step, the basic component data of the sponge titanium electrode is obtained by drilling electrode debris and measuring multiple component indicators. The subsequent volatile weight determination, titanium ingot and ash composition determination, and volatile composition calculation are gradually derived to obtain volatile-related data. Each step is interrelated and progressive, and together they achieve the measurement of the volatiles of sponge titanium.

[0015] As a preferred embodiment of the present invention, the specific steps of S3 are:

[0016] S31, installing the electrode on the jacket, and weighing to obtain the weight of the electrode plus the jacket A1;

[0017] S32. Place a layer of titanium sponge fine particles with known composition on the bottom of the copper crucible. The weight of the titanium sponge fine particles is A2.

[0018] S33, respectively installing the jacket and the copper crucible on a vacuum consumable furnace, cleaning the furnace before loading, connecting the positive and negative poles of the power supply, pumping the negative pressure until the vacuum degree meets the requirement, turning on the current adjustment button, and generating an arc between the consumable electrode and the copper crucible at a certain voltage, so that the consumable electrode melts, and the molten droplets fall onto the surface of the cold crucible and solidify;

[0019] S34. After smelting, cool for a period of time, remove the copper crucible and the remaining electrode, weigh the titanium ingot in the copper crucible (A3), which is a mixture of titanium sponge added to the bottom of the crucible and the molten droplets melted from the electrode, and the jacket and the remaining electrode (A4). Clean the residual material in the furnace and crucible, and weigh the ash content of the furnace wall and the copper crucible (A5).

[0020] S35. Obtain the electrode smelting weight A6, volatile matter weight A7, and volatile matter proportion A8 by calculation, wherein the electrode smelting weight A6=A1-A4, the volatile matter weight A7=A1+A2-A3-A4-A5, and the volatile matter proportion A8=A7 / A6.

[0021] This setting utilizes a gravimetric method to precisely measure the weight of the electrode and jacket (A1), the weight of the titanium sponge particles at the bottom of the crucible (A2), the weight of the titanium ingot (A3), the weight of the jacket and residual electrode (A4), and the weight of the furnace wall and crucible ash (A5). Based on the principle of conservation of mass, the electrode smelting weight (A6), the volatile weight (A7), and the volatile content (A8) are calculated. The electrode is arc-melted in a vacuum consumable furnace to form a titanium ingot. During this process, volatiles are released. The precise measurement and calculation of these weights allows for quantification of the volatile content.

[0022] As a preferred embodiment of the present invention, the specific steps of step S4 are:

[0023] S41, peeling the titanium ingot;

[0024] S42, collecting the peeled material and weighing it as A9;

[0025] S43, weighing the core of the titanium ingot A10;

[0026] S44. Measure the composition of the titanium ingot core, peeling material and ash respectively. The composition analysis indicators are consistent with the electrode indicators.

[0027] This setting is designed for titanium ingot and ash composition determination. The titanium ingot is first peeled and separated into the peeled material and the core. The components of each are then collected and weighed, and the ash composition is measured simultaneously. This is because during the smelting process, the surface and core of the titanium ingot may have different levels of contact with the external environment, resulting in uneven distribution of components. By separately measuring the composition of the peeled material, core, and ash, combined with electrode composition data, a more comprehensive and accurate analysis of the elemental composition of each component can be achieved, providing detailed and accurate data for volatile component calculations.

[0028] As a preferred embodiment of the present invention, in step S5, the content of each element in the volatile matter = electrode smelting weight × element content in the electrode + weight of sponge titanium at the bottom of the crucible × element content in sponge titanium - ash weight × element content in ash - peeling material weight × element content in peeling material - titanium ingot core weight × element content in titanium ingot core.

[0029] This setting is based on the law of conservation of matter. In the calculation of volatile components, the weight of the electrode melt, the elemental content in the electrode, the weight of the titanium sponge at the bottom of the crucible, the elemental content of the titanium sponge, the weight of the ash, the elemental content in the ash, the weight of the peeled material, the elemental content in the peeled material, and the weight and elemental content of the titanium ingot core are comprehensively calculated. In this way, the elemental content of each component of the titanium sponge material involved in the entire measurement process is integrated and calculated, offsetting the elemental influence of other components, thereby deriving the accurate content of each element in the volatile matter.

[0030] As a preferred embodiment of the present invention, in step S2, the method of drilling the debris is as follows: sampling is performed by drilling just above 5 mm from the end of the electrode, and then drilling is performed just in front at intervals of 5 mm, and the drilling is performed alternately in sequence.

[0031] This setting is designed to drill debris from the electrode, alternating between drilling directly above and directly in front of the electrode tip at a distance of 5 mm. This positioning ensures that samples are obtained from different locations on the electrode, avoiding the lack of representativeness caused by sampling from a single location. By alternating sampling at multiple locations on the electrode, the overall composition distribution of the electrode can be more comprehensively reflected, ensuring that the mixed debris more accurately represents the electrode's composition, thereby ensuring the accuracy of subsequent composition testing results.

[0032] As a preferred embodiment of the present invention, in step S2, the composition index is measured as follows: the Cl element sample is dissolved with hydrofluoric acid, oxidized with nitric acid, fluoride ions are complexed with boric acid, silver nitrate is added to form a silver chloride precipitate, and its absorbance is measured at 430 nm on a spectrophotometer; C is measured on a high-frequency infrared carbon-sulfur analyzer; O, N, and H are measured on an oxygen-nitrogen-hydrogen combined analyzer; Fe, Si, Mn, Mg, Ni, Cr, Sn, and Al are dissolved with hydrofluoric acid, oxidized with nitric acid, and measured using ICP after constant volume.

[0033] This setting uses specific measurement methods for different component indicators based on the chemical and physical properties of each element. For example, Cl utilizes its chemical reaction properties with reagents such as hydrofluoric acid, nitric acid, boric acid, and silver nitrate to determine its content by forming a silver chloride precipitate and measuring its absorbance at a specific wavelength. C utilizes the principle of a high-frequency infrared carbon-sulfur analyzer, converting carbon to carbon dioxide at high temperatures, and its content is determined by infrared detection. O, N, and H are measured using an oxygen-nitrogen-hydrogen combined analyzer based on gas analysis principles. Elements such as Fe, Si, Mn, Mg, Ni, Cr, Sn, and Al utilize the strong oxidizing properties of hydrofluoric acid and nitric acid to dissolve the sample, followed by elemental analysis using ICP technology, determining their content based on the characteristic spectra produced by each element's excitation in the plasma.

[0034] As a preferred embodiment of the present invention, a measuring device for measuring the volatile matter of sponge titanium is also included, including a mixer, a sample pressing chamber, a measuring cylinder, a hydraulic press, and a sand mill.

[0035] The measurement setup includes a mixer, sample pressing chamber, graduated cylinder, hydraulic press, and sand mill. Each device performs different functions and works in conjunction with each other during the measurement process. The mixer is used for preliminary sample preparation and homogenization; the sample pressing chamber allows for sample reduction; the graduated cylinder measures bulk density; the hydraulic press compresses the sample into electrodes; and the sand mill polishes the electrodes. Together, these devices form a complete operating platform, from sample preparation to electrode fabrication, providing the necessary hardware support for the initial sample processing required for volatile matter measurements in titanium sponge.

[0036] As a preferred embodiment of the present invention, it also includes a sponge titanium electrode sampling mechanism, which includes a bracket, clamping plates are installed on both sides of the bracket, the clamping plates clamp the two ends of the electrode and are locked and fixed by tightening bolts, a horizontal screw component is installed on the top of the bracket, a punching cylinder is installed on the slider of the bracket, and a punching head is installed on the bottom output shaft of the punching cylinder.

[0037] This titanium sponge electrode sampling mechanism utilizes a combination of a bracket, clamping plate, jacking bolts, a screw assembly, a punching cylinder, and a punching head to achieve stable electrode clamping and precise sampling. The clamping plate and jacking bolts secure the electrode, ensuring its stable position during sampling. The screw assembly and slider precisely adjust the punching cylinder's position, enabling sampling at different electrode locations. The punching cylinder drives the punching head to drill into the electrode, obtaining the desired debris sample.

[0038] As a preferred solution of the present invention, a collecting tank is provided at the lower portion of the bracket.

[0039] This setting sets up a collection trough at the bottom of the bracket. The principle is that debris will be generated during the sampling process. The collection trough can collect these debris in time to prevent the debris from scattering, keep the working environment clean, and avoid the loss of debris affecting the integrity and accuracy of the sample, ensuring that all collected debris are used for component detection.

[0040] As a preferred embodiment of the present invention, it also includes a device for measuring the weight of volatile matter, including a jacket, a copper crucible, and a vacuum consumable furnace. A spring is installed on the inner side of the jacket, an electrode is placed in the jacket and clamped in place by the spring, the jacket is placed in the copper crucible, and placed in the vacuum consumable furnace.

[0041] This setup is used in volatile matter weight determination devices. A spring clip inside the jacket clamps and positions the electrode, securing it within the copper crucible and maintaining stability during melting in a vacuum consumable furnace. The crucible collects the molten electrode droplets, while the vacuum consumable furnace provides the vacuum environment and arc conditions necessary for melting. The coordinated operation of these components ensures stable electrode melting in a vacuum environment, providing reliable experimental conditions for accurate volatile matter weight measurement.

[0042] Compared with the prior art, the present invention has the following beneficial effects:

[0043] 1. This method for measuring titanium sponge volatiles, by accurately measuring the content and composition of volatiles in titanium sponge, enables in-depth analysis of factors affecting the generation of volatiles during the production process, thereby providing reliable data support for optimizing process parameters for magnesium thermal production of titanium sponge. For example, based on the measurement results, the conditions of key processes such as reduction and distillation can be adjusted in a targeted manner, and process routes for producing low-volatile titanium sponge products can be explored, thereby reducing the generation of volatiles at the source and improving product quality and production efficiency.

[0044] 2. This method for measuring the volatile content of titanium sponge can accurately measure the volatile content of batches of titanium sponge, providing detailed data for the vacuum melting process of titanium ingots. Operators can rationally adjust melting equipment parameters such as vacuum level, voltage, and current based on the weight, proportion, and elemental content of the volatile content to ensure a stable melting process, avoid equipment failures and product quality defects caused by volatile content, and improve the melting quality and yield of titanium ingots.

[0045] 3. In the past, due to the inability to accurately control the volatile content of titanium sponge, downstream customers frequently encountered problems such as equipment corrosion and smelting anomalies during use, resulting in an increase in customer complaints. This invention achieves accurate measurement and effective control of the volatile content of titanium sponge, which can significantly reduce customer complaints caused by volatile content issues, lower the cost of handling after-sales issues for enterprises, including equipment maintenance, product returns, technical support, etc., and improve the economic benefits and market reputation of enterprises.

[0046] 4. This titanium sponge volatile content measurement method allows for targeted screening and provision of products that meet customer requirements based on the volatile content measurement data. Whether for high-end applications with strict limits on volatile content or for customers with specific elemental composition requirements, we can provide precisely matched titanium sponge products, better serving downstream customers and enhancing customer satisfaction and market competitiveness. BRIEF DESCRIPTION OF THE DRAWINGS

[0047] Figure 1 It is a schematic diagram of the process of the present invention;

[0048] Figure 2 Schematic diagram of the internal structure of the vacuum consumable furnace in the present invention;

[0049] Figure 3 Schematic diagram of the internal structure of the jacket in the present invention;

[0050] Figure 4 Schematic diagram of the structure of the titanium sponge electrode sampling mechanism of the present invention;

[0051] The meaning of each number in the figure is:

[0052] 1. Vacuum consumable furnace; 2. Sample pressing chamber; 3. Measuring cylinder; 4. Hydraulic press; 5. Sand grinder; 6. Jacket; 61. Shrapnel; 7. Copper crucible; 8. Vacuum consumable furnace; 9. Sponge titanium electrode sampling mechanism; 91. Bracket; 92. Clamping plate; 93. Jacking bolt; 94. Screw rod assembly; 95. Punching cylinder; 951. Punching head; 96. Collection tank. DETAILED DESCRIPTION

[0053] The following will clearly and completely describe the technical solutions in the embodiments of the present invention in conjunction with the accompanying drawings. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without making creative efforts are within the scope of protection of the present invention.

[0054] The present invention provides a method for measuring the volatile matter of titanium sponge. Figure 1 As shown, the following steps are included:

[0055] S1. Sample preparation: The sample taken out in step 1 is initially reduced to approximately 4 kg, and further reduced in the sample pressing chamber 2 to obtain two 1 kg samples. The samples are placed in a graduated cylinder 3 and compacted to measure the bulk density. The average value is taken, and the electrodes are then pressed into an electrode using a hydraulic press 4, and the edges and corners of the electrodes are smoothed using a sand grinder 5.

[0056] S2. Detection of the composition of the titanium sponge electrode: Drill chips at the required points on the titanium sponge electrode, mix them thoroughly and measure the composition indicators, which include Fe, Si, Cl, C, N, O, Mn, Mg, H, Ni, Cr, Sn, and Al;

[0057] S3. Determination of volatile matter weight;

[0058] S4, titanium ingot, determination of ash composition;

[0059] S5. Calculation of volatile components.

[0060] This claim constructs the overall process framework for the measurement of sponge titanium volatiles. In the sample preparation stage, the sample is taken out and initially reduced by using a mixer 1, and then reduced again in the sample pressing chamber 2 to process the sample to an appropriate weight to ensure the representativeness of the sample and the feasibility of subsequent operations; the bulk density is measured using a measuring cylinder 3, the sample is pressed into an electrode by a hydraulic press 4, and finally the electrode edges are polished flat on a sand mill 5 to provide a standard sample morphology for subsequent component detection and volatile determination. In the component detection step, the basic component data of the sponge titanium electrode is obtained by drilling debris at the required points on the sponge titanium electrode and measuring a variety of component indicators. Subsequent volatile weight determination, titanium ingot and ash component determination, and volatile component calculation are used to gradually derive volatile-related data. Each step is interrelated and progressive, and together achieves the measurement of sponge titanium volatiles. It provides a systematic and comprehensive operating procedure for the measurement of volatile matter in titanium sponge, ensuring that the measurement process is standardized and orderly. It can obtain data from multiple dimensions, laying the foundation for the accurate determination of volatile content and composition, avoiding result deviations caused by missing or non-standard measurement processes, and improving the reliability and accuracy of measurements.

[0061] In this embodiment, Figure 2 As shown, the specific steps of S3 are:

[0062] S31, installing the electrode on the jacket 6, and weighing to obtain the weight A1 of the electrode plus the jacket;

[0063] S32, placing a layer of titanium sponge fine particles with known composition index on the bottom of the copper crucible 7, the titanium sponge fine particles weighing A2;

[0064] S33, respectively install the jacket 6 and the copper crucible 7 on the vacuum consumable furnace 8, clean the furnace before loading, connect the positive and negative poles of the power supply, pump the negative pressure until the vacuum degree meets the requirement, turn on the current adjustment button, and generate an arc between the consumable electrode and the copper crucible 7 at a certain voltage, so that the consumable electrode melts, and the molten droplets fall onto the surface of the cold crucible and solidify;

[0065] S34, after smelting, cool for a period of time, remove the copper crucible 7 and the remaining electrode, weigh the titanium ingot in the copper crucible 7 to be A3, the titanium ingot is a mixture of sponge titanium added to the bottom of the crucible and the molten droplets melted from the electrode, the jacket 6 and the remaining electrode to be A4, clean the residual material in the furnace and crucible, and weigh the ash content of the furnace wall and the copper crucible 7 to be A5;

[0066] S35. Obtain the electrode smelting weight A6, volatile matter weight A7, and volatile matter proportion A8 by calculation, wherein the electrode smelting weight A6=A1-A4, the volatile matter weight A7=A1+A2-A3-A4-A5, and the volatile matter proportion A8=A7 / A6.

[0067] The volatile matter weight determination process utilizes a gravimetric method to precisely measure the weight (A1) of the electrode plus jacket (assembly of the electrode and jacket, obtained by mounting the electrode on the jacket 6); the weight (A2) of titanium sponge particles of known composition placed on the bottom of the copper crucible 7; the weight (A3) of the titanium ingot in the copper crucible 7; the weight (A4) of the jacket 6 and remaining electrode; and the weight (A5) of the ash in the furnace wall and copper crucible 7. Based on the principle of conservation of mass, the electrode smelting weight (A6), volatile matter weight (A7), and volatile matter percentage (A8) are calculated. The jacket 6 and copper crucible 7 are then mounted on a vacuum consumable furnace 8, and the electrode is melted by arc melting to form a titanium ingot. During this process, volatile matter escapes. The precise measurement and calculation of these weights allows for quantification of the volatile matter weight. It provides a scientific and rigorous method for determining the weight of volatile matter. Through multiple precise weighings and strict calculation logic, it can accurately determine the weight and proportion of volatile matter in sponge titanium during the smelting process. It provides key data for evaluating the volatility characteristics of sponge titanium, helps to gain a deeper understanding of the volatilization law of sponge titanium during vacuum melting, and thus provides strong data support for production process optimization.

[0068] Specifically, the specific steps of step S4 are:

[0069] S41, peeling the titanium ingot;

[0070] S42, collecting the peeled material and weighing it as A9;

[0071] S43, weighing the core of the titanium ingot A10;

[0072] S44. Measure the composition of the titanium ingot core, peeling material and ash respectively. The composition analysis indicators are consistent with the electrode indicators.

[0073] To determine the composition of titanium ingots and ash, the titanium ingots are first peeled and divided into two parts: the peeled material and the core. These parts are then collected and weighed, and their composition is measured. The ash composition is also measured. This is based on the fact that during the smelting process, the surface and core of the titanium ingot may have different degrees of contact with the external environment, resulting in uneven distribution of components. By separately measuring the composition of the peeled material, core, and ash, combined with electrode composition data, the elemental composition of each part can be analyzed more comprehensively and accurately, providing detailed and accurate data for the calculation of volatile components. This ensures that the determination of the titanium ingot and ash composition is more detailed and accurate, avoiding errors in the calculation of volatile components caused by incomplete composition measurements. By obtaining compositional information from different parts of the titanium ingot and the ash, the changes in the material of sponge titanium during the smelting process can be more accurately understood, providing a reliable data basis for accurately calculating the content of each element in the volatile matter, and improving the accuracy and reliability of the entire measurement method.

[0074] Furthermore, in step S5, the content of each element in the volatile matter = electrode smelting weight × element content in the electrode + weight of sponge titanium at the bottom of the crucible × element content in sponge titanium - ash weight × element content in ash - peeling material weight × element content in peeling material - titanium ingot core weight × element content in titanium ingot core.

[0075] Based on the law of conservation of matter, the volatile composition calculation incorporates data such as the electrode smelting weight, elemental content in the electrode, weight of the titanium sponge at the bottom of the crucible, elemental content in the titanium sponge, ash weight, elemental content in the ash, weight of the peeled material, elemental content in the peeled material, and weight of the titanium ingot core, elemental content in the titanium ingot core. This method integrates the elemental content of each component of the titanium sponge throughout the measurement process, offsetting the influence of elements from other components to accurately determine the content of each element in the volatiles. This precise calculation of the elemental content of each element in the titanium sponge volatiles enables detailed analysis of the volatile composition, providing accurate data for in-depth research into the properties of the volatiles in titanium sponge. Accurate composition calculation helps companies understand the specific composition of titanium sponge volatiles, enabling targeted improvements to production processes, reducing the generation of harmful volatiles, and improving the quality of titanium sponge products and the environmental friendliness of the production process.

[0076] Furthermore, in step S2, the method of drilling the debris points is as follows: sampling is performed by drilling just above the electrode end at a distance of 5 mm, and then drilling is performed just in front at intervals of 5 mm, and the drilling is performed alternately in sequence.

[0077] In the design of the electrode drilling point for debris, the method of alternating drilling is adopted, which is 5 mm away from the end of the electrode and directly in front of it. This point design is to ensure that samples are obtained from different positions of the electrode to avoid the lack of representativeness of the sample due to a single sampling position. By alternately sampling at multiple positions of the electrode, the overall composition distribution of the electrode can be more comprehensively reflected, so that the mixed debris can more truly represent the composition of the electrode, thereby ensuring the accuracy of subsequent composition test results. The representativeness of the electrode composition test sample is improved, so that the measured composition index can more accurately reflect the true composition of the sponge titanium electrode. Avoid inaccurate composition test results due to sampling deviation, provide reliable basic data for subsequent volatile composition calculations, ensure the accuracy and effectiveness of the composition data throughout the measurement process, and improve the credibility of the volatile content measurement results of sponge titanium.

[0078] Furthermore, in step S2, the method of measuring the component indicators is as follows: the Cl element sample is dissolved with hydrofluoric acid, oxidized with nitric acid, the fluoride ion is complexed with boric acid, silver nitrate is added to form a silver chloride precipitate, and its absorbance is measured at 430nm on a spectrophotometer; C is measured on a high-frequency infrared carbon-sulfur analyzer; O, N, and H are measured on an oxygen-nitrogen-hydrogen combined analyzer; Fe, Si, Mn, Mg, Ni, Cr, Sn, and Al are dissolved with hydrofluoric acid, oxidized with nitric acid, and measured using ICP after constant volume.

[0079] Specific measurement methods are used for different component indicators based on the chemical and physical properties of each element. For example, Cl utilizes its chemical reaction properties with reagents such as hydrofluoric acid, nitric acid, boric acid, and silver nitrate to determine its content by forming a silver chloride precipitate and measuring its absorbance at a specific wavelength. C utilizes the principle of a high-frequency infrared carbon-sulfur analyzer, converting carbon to carbon dioxide at high temperatures, and its content is determined by infrared detection. O, N, and H are measured using an oxygen-nitrogen-hydrogen combined analyzer based on gas analysis principles. Elements such as Fe, Si, Mn, Mg, Ni, Cr, Sn, and Al are analyzed using the highly oxidizing properties of hydrofluoric acid and nitric acid to dissolve the sample. ICP inductively coupled plasma analysis is then used to determine the content based on the characteristic spectra produced by each element excited in the plasma. This ensures highly accurate and professional measurement of the various component indicators in titanium sponge electrodes. Selecting appropriate measurement methods based on the characteristics of different elements can give full play to the advantages of various analytical techniques, accurately determine the content of each element, provide reliable data support for the calculation of volatile components and overall measurement results, improve the scientificity and effectiveness of the measurement method, and enable the measurement results to accurately reflect the composition information of sponge titanium.

[0080] Furthermore, the invention also includes a measuring device for measuring the volatile matter of sponge titanium, including a mixer 1, a sample pressing chamber 2, a measuring cylinder 3, a hydraulic press 4, and a sand mill 5.

[0081] The measuring device includes a mixer 1, a sample pressing chamber 2, a graduated cylinder 3, a hydraulic press 4, and a sand mill 5. Each device performs a different function in the measurement process and works in conjunction with each other. Mixer 1 is used for preliminary sample processing to ensure uniform mixing; sample pressing chamber 2 reduces the sample; graduated cylinder 3 is used to measure bulk density; hydraulic press 4 presses the sample into electrodes; and sand mill 5 polishes the electrodes. Together, these devices form a complete operating platform from sample preparation to electrode preparation, providing the necessary hardware support for the initial sample processing for titanium sponge volatile content measurements. This provides comprehensive equipment support for the sample preparation phase of titanium sponge volatile content measurements, ensuring smooth and efficient sample processing, as well as standardized and consistent sample processing, thereby improving the reliability and repeatability of measurement results. Each device has a clear division of labor and works in tandem, meeting various sample processing requirements during the measurement process and making the entire measurement process more standardized and professional.

[0082] Further, such as Figure 4 As shown, it also includes a sponge titanium electrode sampling mechanism 9, which includes a bracket 91. Clamping plates 92 are installed on both sides of the bracket 91. The clamping plates 92 clamp the two ends of the electrode and are locked and fixed by tightening bolts 93. A horizontal screw component 94 is installed on the top of the bracket 91, and a punching cylinder 95 is installed on the slider of the bracket 91. The bottom output shaft of the punching cylinder 95 is installed with a punching head 951.

[0083] The titanium sponge electrode sampling mechanism 9 achieves stable electrode clamping and precise sampling through the combined design of a bracket 91, a clamping plate 92, a tightening bolt 93, a screw assembly 94, a punching cylinder 95, and a punching head 951. The clamping plate 92 and the tightening bolt 93 are used to secure the electrode, ensuring its stable position during sampling. The screw assembly 94 and the slider precisely adjust the position of the punching cylinder 95, enabling sampling at different electrode locations. The punching cylinder 95 drives the punching head 951 to drill the electrode, thereby obtaining the required debris sample. This improves the accuracy and efficiency of electrode sampling, ensuring the quality and representativeness of the samples taken. Through stable clamping and precise positioning, samples can be accurately obtained at different electrode locations, avoiding sampling inaccuracies caused by manual operation errors. Furthermore, mechanized sampling is more efficient than manual operation, quickly obtaining sufficient samples for component testing, ensuring the smooth progress of the measurement process and improving the efficiency and quality of the entire measurement process.

[0084] Furthermore, a collecting tank 96 is provided at the lower portion of the bracket 91 .

[0085] A collection trough 96 is provided at the bottom of bracket 91. This is based on the principle that debris generated during the sampling process can be promptly collected by the collection trough 96, preventing it from scattering and maintaining a clean working environment. This also prevents debris loss from affecting sample integrity and accuracy, ensuring that all collected debris is used for component analysis. This effectively collects debris generated during the electrode sampling process, ensuring sample integrity and avoiding sample insufficiency or compositional deviations caused by debris loss, thereby improving the accuracy of component analysis results. Furthermore, this maintains a clean and orderly working environment, facilitating subsequent measurements for operators, improving work efficiency, and reducing interference from environmental factors on the measurement process.

[0086] Further, such as Figure 2 、 Figure 3 As shown, it also includes a device for measuring the weight of volatile matter, including a jacket 6, a copper crucible 7, and a vacuum consumable furnace 8. A spring 61 is installed on the inner side of the jacket 6. An electrode is placed in the jacket 6 and clamped in place by the spring 61. The jacket 6 is placed in the copper crucible 7 and placed in the vacuum consumable furnace 8.

[0087] In the device for measuring the weight of volatile matter, the spring piece 61 on the inner side of the jacket 6 can clamp and position the electrode, ensuring that the electrode is fixed in position in the copper crucible 7 and remains stable during smelting in the vacuum consumable furnace 8; the copper crucible 7 is used to receive the molten droplets after the electrode is melted; the vacuum consumable furnace 8 provides a vacuum environment and arc conditions required for smelting. Through the coordinated work of various components, the electrode can be stably smelted in a vacuum environment, providing reliable experimental conditions for accurately measuring the weight of volatile matter. It ensures that the electrode can be stably melted during the volatile matter weight measurement process, improving the accuracy and reliability of the measurement results. Stable electrode positioning and suitable smelting equipment can ensure that the electrode performs as expected during the smelting process, avoid measurement errors caused by problems such as electrode shaking and displacement, make the volatile matter weight measurement more accurate, and provide reliable data guarantee for the volatile matter measurement of sponge titanium.

[0088] Finally, it should be noted that the vacuum consumable furnace vacuum consumable furnace 1 and other components in this embodiment, the electronic components in the above parts are all universal standard parts or components known to those skilled in the art, and their structures and principles can be known to those skilled in the art through technical manuals or through conventional experimental methods. In the idle part of this device, all the above electrical components are connected respectively through wires. The specific connection means should refer to the working sequence between the electrical components in the above working principle to complete the electrical connection, which are all well-known technologies in the art.

[0089] The above shows and describes the basic principles, main features, and advantages of the present invention. Those skilled in the art should understand that the present invention is not limited to the above embodiments. The above embodiments and descriptions are merely preferred examples of the present invention and are not intended to limit the present invention. Various changes and improvements may be made to the present invention without departing from the spirit and scope of the present invention. Such changes and improvements fall within the scope of the present invention. The scope of protection claimed in the present invention is defined by the appended claims and their equivalents.

Claims

1. A method for measuring volatile matter of titanium sponge, characterized in that: The steps include: S1. Sample preparation: The sample taken out in (1) is initially reduced to about 4 kg, and then reduced again in the sample pressing chamber (2) to obtain two 1 kg samples, which are placed in a measuring cylinder (3) and vibrated to measure the bulk density, and the average value is taken. Then, the samples are pressed into electrodes on a hydraulic press (4), and the edges and corners of the electrodes are smoothed on a sand grinder (5); S2. Detection of the composition of the titanium sponge electrode: Drill chips at the required points on the titanium sponge electrode, mix them thoroughly and measure the composition indicators, which include Fe, Si, Cl, C, N, O, Mn, Mg, H, Ni, Cr, Sn, and Al; S3. Determination of volatile matter weight; S4, titanium ingot, determination of ash composition; S5. Calculation of volatile components.

2. The method for measuring volatile matter of titanium sponge according to claim 1, wherein: The specific steps of S3 are: S31, installing the electrode on the jacket (6), and weighing to obtain the weight A1 of the electrode plus the jacket; S32, placing a layer of titanium sponge fine particles with known composition index on the bottom of the copper crucible (7), the titanium sponge fine particles weighing A2; S33, respectively install the jacket (6) and the copper crucible (7) on the vacuum consumable furnace (8), clean the furnace before loading, connect the positive and negative poles of the power supply, pump the negative pressure until the vacuum degree meets the requirements, turn on the current adjustment button, and generate an arc between the consumable electrode and the copper crucible (7) at a certain voltage, so that the consumable electrode melts and the molten droplets fall onto the surface of the cold crucible and solidify; S34, after smelting, cool for a period of time, take out the copper crucible (7) and the residual electrode, weigh the titanium ingot in the copper crucible (7) to be A3, the titanium ingot is a mixture of sponge titanium added to the bottom of the crucible and the molten droplets melted from the electrode, the jacket (6) and the residual electrode weigh A4, clean the residual material in the furnace and crucible, and weigh the ash weight of the furnace wall and the copper crucible (7) to be A5; S35. Obtain the electrode smelting weight A6, volatile matter weight A7, and volatile matter proportion A8 by calculation, wherein the electrode smelting weight A6=A1-A4, the volatile matter weight A7=A1+A2-A3-A4-A5, and the volatile matter proportion A8=A7 / A6.

3. The method for measuring volatile matter of titanium sponge according to claim 1, wherein: The specific steps of step S4 are: S41, peeling the titanium ingot; S42, collecting the peeled material and weighing it as A9; S43, weighing the core of the titanium ingot A10; S44. Measure the composition of the titanium ingot core, peeling material and ash respectively. The composition analysis indicators are consistent with the electrode indicators.

4. The method for measuring volatile matter of titanium sponge according to claim 1, wherein: In step S5, the content of each element in the volatile matter = electrode smelting weight × element content in the electrode + weight of sponge titanium at the bottom of the crucible × element content in sponge titanium - ash weight × element content in ash - peeling material weight × element content in peeling material - titanium ingot core weight × element content in titanium ingot core.

5. The method for measuring volatile matter of titanium sponge according to claim 1, wherein: In step S2, the method of drilling the debris points is as follows: sampling is performed by drilling just above the electrode end at a distance of 5 mm, and then drilling is performed just in front at intervals of 5 mm, and the drilling is performed alternately in sequence.

6. The method for measuring volatile matter of titanium sponge according to claim 1, wherein: In step S2, the method of measuring the component indicators is as follows: the Cl element sample is dissolved with hydrofluoric acid, oxidized with nitric acid, fluoride ions are complexed with boric acid, silver nitrate is added to form a silver chloride precipitate, and its absorbance is measured at 430 nm on a spectrophotometer; C is measured on a high-frequency infrared carbon-sulfur analyzer; O, N, and H are measured on an oxygen-nitrogen-hydrogen combined analyzer; Fe, Si, Mn, Mg, Ni, Cr, Sn, and Al are dissolved with hydrofluoric acid, oxidized with nitric acid, and measured using ICP after constant volume.

7. The method for measuring volatile matter of titanium sponge according to claim 1, wherein: Also included is a measuring device for a method of measuring volatile matter in titanium sponge, comprising a mixer (1), a sample pressing chamber (2), a measuring cylinder (3), a hydraulic press (4), and a sand mill (5).

8. The method for measuring volatile matter of titanium sponge according to claim 1, wherein: The invention also includes a titanium sponge electrode sampling mechanism (9), which includes a bracket (91), clamping plates (92) are installed on both sides of the bracket (91), the clamping plates (92) clamp the two ends of the electrode and are locked and fixed by tightening bolts (93), a horizontal screw rod component (94) is installed on the top of the bracket (91), a punching cylinder (95) is installed on the slider of the bracket (91), and a punching head (951) is installed on the bottom output shaft of the punching cylinder (95).

9. The method for measuring volatile matter of titanium sponge according to claim 8, characterized in that: A collecting trough (96) is provided at the lower portion of the bracket (91).

10. The method for measuring volatile matter of titanium sponge according to claim 2, characterized in that: It also includes a device for measuring the weight of volatile matter, including a jacket (6), a copper crucible (7), and a vacuum consumable furnace (8). A spring (61) is installed on the inner side of the jacket (6). An electrode is placed in the jacket (6) and is clamped and positioned by the spring (61). The jacket (6) is placed in the copper crucible (7) and placed in the vacuum consumable furnace (8).

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