Method for producing high-yield Group 5 transition metal-containing precursors for thin film formation

Abstract

This provides a method for producing a precursor for forming a Group 5 transition metal-containing thin film with high yield. [Solution] The present invention provides a method for producing a high-yield Group 5 transition metal-containing thin film precursor, comprising the steps of: reacting a Group 5 transition metal supplying material and a solvent to form a complex compound; and reacting the complex compound with a ligand or ligand salt to form a Group 5 transition metal compound. This method increases the synthesis yield and productivity of the precursor compound, thereby improving the efficiency of the thin film formation process.

Description

Technical Field

[0001] The present invention relates to a method for producing a precursor for forming a high-yield Group 5 transition metal-containing thin film, and particularly to a method for producing a precursor for forming a high-yield Group 5 transition metal-containing thin film capable of obtaining a Group 5 transition metal compound for a precursor at a high yield as compared with conventional synthesis methods.

Background Art

[0002] Thin films containing Group 5 transition metals such as vanadium (V), niobium (Nb), and tantalum (Ta) are applied to elements that require high dielectric properties such as DRAM and CMOS. Such Group 5 transition metal-containing thin films can be produced by a thin film forming process using various metal precursors.

[0003] Such precursor compounds for forming a Group 5 transition metal-containing thin film are produced by the reaction of a compound for supplying a Group 5 transition metal as a central metal and a compound constituting a ligand. In this case, there is a problem that the yield is difficult to exceed 40%. Of course, if the yield is low in the synthesis process of the precursor compound, the purity can be increased by post-processes such as purification. However, if the purity should be increased by such post-processes, more energy and processes are required, leading to a decrease in the overall productivity of the thin film forming process.

[0004] Therefore, it is necessary to produce a high-quality precursor compound by increasing the yield in the process of synthesizing the precursor compound, thereby improving the productivity of the thin film forming process.

Summary of the Invention

Problems to be Solved by the Invention

[0005] The present invention has been devised to solve such problems of the prior art, and an object thereof is to provide a production method capable of producing a Group 5 transition metal compound used as a precursor for forming a Group 5 transition metal thin film at a high yield.

[0006] Furthermore, the objective is to provide a method that can effectively reduce impurities in precursors in order to purify the Group 5 transition metal compounds. [Means for solving the problem]

[0007] The present invention provides a method for producing a high-yield Group 5 transition metal-containing thin film precursor to solve the above problems, and is characterized by comprising the steps of: reacting a Group 5 transition metal supplying material and a solvent to form a complex compound; and reacting the complex compound with a ligand or ligand salt to form a Group 5 transition metal compound.

[0008] In this case, the solvent may be selected from compounds containing lone pairs of electrons.

[0009] Furthermore, the solvent may be a compound containing either a nitrogen atom (N) or an oxygen atom (O), or both.

[0010] Furthermore, the solvent may be any of the following, or a mixture thereof: tetrahydrofuran (THF), dimethoxyethane (DME), diethyl ether, dimethoxymethane (DMM), 1,4-dioxane, pyridine, 2,2'-bipyridine, acetonitrile, or tetramethylethylenediamine.

[0011] Furthermore, the step of forming the group 5 transition metal compound may involve reacting the complex compound with a ligand or ligand salt in the presence of at least one solvent, which includes both polar and nonpolar solvents.

[0012] Furthermore, the yield of the group 5 transition metal compound obtained by the step of forming the group 5 transition metal compound may be 40% or more.

[0013] Furthermore, the yield improvement rate of the group 5 transition metal compound obtained by the step of forming the group 5 transition metal compound may be 100% or more.

[0014] The process may further include a step of heat-treating the group 5 transition metal compound obtained by the step of forming the group 5 transition metal compound at a heat treatment temperature.

[0015] In this case, the heat treatment step may be performed at a heat treatment temperature of 80 to 240°C for 0.01 to 48 hours.

[0016] Furthermore, the heat treatment step may be performed after raising the temperature from room temperature to the heat treatment temperature at a heating rate of 0.1 to 10°C / minute.

[0017] The process may also include a step of purifying the group 5 transition metal compound at least once before or after heat treatment.

[0018] Furthermore, in the purification step, the group 5 transition metal compound may be purified by vacuum distillation.

[0019] Furthermore, the heat treatment step may be performed in the following ways: i) heat treatment in a container on which the group 5 transition metal compound is supported; ii) heat treatment of the group 5 transition metal compound in a transfer section where it is moved from one container to another; or iii) heat treatment of the group 5 transition metal compound both in the container on which the group 5 transition metal compound is supported and in a transfer section where it is moved from one container to another. [Effects of the Invention]

[0020] The method for producing a high-yield Group 5 transition metal-containing thin film precursor according to the present invention has the effect of synthesizing Group 5 transition metal compounds used as precursors for forming Group 5 transition metal thin films in high yield.

[0021] In addition, heat treatment of the Group 5 transition metal compound exhibits the effect that impurities in the precursor can be effectively reduced to produce a high-purity Group 5 transition metal compound.

Brief Description of Drawings

[0022] [Figure 1] It is the TGA analysis result of V(EMA)4 produced by Synthesis Example 1. [Figure 2] It is the DSC analysis result of V(EMA)4 produced by Synthesis Example 1. [Figure 3] It is the inductively coupled plasma mass spectrometry result of the sample according to Example 1-1.

Modes for Carrying Out the Invention

[0023] Hereinafter, the present invention will be described in more detail. Terms or words used in this specification and the claims should not be construed as being limited to their ordinary or dictionary meanings, and the inventor should be in accordance with the principle that the concept of the terms can be appropriately defined in order to explain his invention in the best way, and should be construed in a meaning and concept consistent with the technical idea of the present invention.

[0024] The method for producing a precursor for forming a high-yield Group 5 transition metal-containing thin film according to the present invention applies an improved manufacturing process capable of increasing the synthesis yield of the Group 5 transition metal compound used as the precursor for forming the Group 5 transition metal-containing thin film and improving productivity.

[0025] Specifically, the method for producing a precursor for forming a high-yield Group 5 transition metal-containing thin film is an improved manufacturing method for increasing the synthesis yield of a Group 5 transition metal compound and reducing impurities in the produced compound, and includes a step of reacting a Group 5 transition metal supply substance and a solvent to form a complex compound, and a step of reacting the complex compound with a ligand or a ligand salt to form a Group 5 transition metal compound.

[0026] Generally, in production methods involving the reaction of a central metal supply material with a ligand salt to form a group 5 transition metal compound, the yield rarely exceeds 40%, which presents a problem in that it is difficult to perform purification steps to increase the purity of the produced group 5 transition metal compound.

[0027] However, the manufacturing method of the present invention significantly increases the synthesis yield of group 5 transition metal compounds by applying a pathway that reacts a ligand salt with a complex compound.

[0028] In other words, applying the manufacturing method of the present invention improves the yield rate to 100% or more. The yield improvement rate is expressed as a percentage of the increase in yield compared to the maximum yield of the group 5 transition metal compound obtained by the conventional synthesis method, i.e., by reacting a group 5 transition metal supply material with a ligand or ligand salt without forming a complex compound.

[0029] In other words, the manufacturing method of the present invention improves the yield compared to conventional synthesis methods by applying a synthesis method in which a group 5 transition metal supply material is produced in the form of a complex compound and then reacted with a ligand salt.

[0030] In addition, separate from the ligand salt, a halide or alkoxy compound of a group 5 transition metal is reacted with a solvent to form a complex compound. By reacting the prepared ligand salt with the complex compound, the target group 5 transition metal compound can be formed. In the process of forming the complex compound, a coordination bond is formed between the transition metal supplier and the solvent molecule during the synthesis of the transition metal compound. The oxidation state of the intermediate thus formed becomes the same as that of the target group 5 transition metal compound, and ultimately, the presence of the coordination bond in the intermediate increases reactivity through the stabilization of the intermediate and its oxidation state.

[0031] In this process, the synthesis yield is affected by the formation of the complex compound. It is preferable to use a solvent selected from compounds containing lone pairs of electrons as the solvent for forming the complex compound. It is also preferable to use a compound containing either a nitrogen atom (N) or an oxygen atom (O), or both.

[0032] Examples of such solvents include tetrahydrofuran (THF), dimethoxyethane (DME), diethyl ether, dimethoxymethane (DMM), 1,4-dioxane, pyridine, 2,2'-bipyridine, acetonitrile, and tetramethylethylenediamine. Alternatively, one or more solvents selected from the above may be used.

[0033] When producing group 5 transition metal compounds using this synthetic route, unlike conventional methods which show very low yields, it was found that the yield improvement rate was more than 100% compared to the highest yield achieved by existing synthesis methods. In other words, when applying the production method of the present invention, it was confirmed that the yield of the group 5 transition metal compound obtained in the step of forming the group 5 transition metal compound was 40% or more.

[0034] Furthermore, to increase the purity of the manufactured Group 5 transition metal compounds, impurities can be reduced by heat treatment after synthesis.

[0035] High-yield Group 5 transition metal compounds can be useful as precursors for thin film formation, but impurities in the compound itself, particularly trace amounts of impurities remaining during the synthesis process, can affect the electrical properties of the thin film. Therefore, the Group 5 transition metal compounds can be purified by applying a heat treatment step at a heat treatment temperature.

[0036] In this case, the heat treatment temperature may be 80 to 240°C, preferably 100 to 210°C, and more preferably 120 to 180°C. Furthermore, the heat treatment can be performed at the heat treatment temperature for 0.01 to 48 hours, preferably 0.01 to 24 hours, and more preferably 0.01 to 12 hours.

[0037] Here, the heat treatment is a process introduced to reduce impurities contained in the object to be heat-treated, and the heat treatment temperature can be understood as the temperature of the object to be heat-treated.

[0038] If the heat treatment temperature is too low and falls outside the above range, the impurity content cannot be reduced below the target value. If it is too high, problems may arise such as a decrease in production efficiency due to vaporization of the compound or thermal decomposition of the precursor compound itself. Furthermore, if the heat treatment time is too short, the impurity content cannot be sufficiently reduced, and if it is too long, it may lead to a decrease in precursor production efficiency due to vaporization of the compound.

[0039] Furthermore, it is preferable that the heat treatment step be performed after raising the temperature from room temperature to the heat treatment temperature at a heating rate of 0.1 to 10°C / minute. The heating rate is also an important process condition in heat treatment, but in a normal heat treatment process, the temperature is raised at a rate of 10°C / minute or less. If the heating rate is too slow, the overall heat treatment process time becomes longer and the process efficiency decreases, so it is preferable to apply the above range of heating rates when performing the heat treatment.

[0040] Furthermore, the heat treatment step can be performed in the following ways: i) heat treatment in a container on which the group 5 transition metal compound is supported; ii) heat treatment of the group 5 metal compound in a transfer section where it is moved from one container to another; or iii) heat treatment of the group 5 transition metal compound both in the container on which the group 5 transition metal compound is supported and in a transfer section where it is moved from one container to another.

[0041] For example, the group 5 transition metal compound can be supported (stored) in a first container (storage container or reaction container) and may also be moved from the first container to another second container (storage container or reaction container). Method i) is a method of heat-treating the group 5 transition metal compound by heating the inside of the first container; Method ii) is a method in which the group 5 transition metal compound supported in the first container is moved to the second container, and the movement section is heated to a high temperature (heat treatment temperature), and the group 5 transition metal compound is heat-treated while moving through the movement section; Method iii) is a method in which the group 5 transition metal compound is heat-treated in the first container, and the movement space in which the group 5 transition metal compound moves to the second container is also heated, and the movement section is heat-treated as well. In this case, the container may be a storage container for storing a precursor, or it may be a reaction container for carrying out a reaction.

[0042] Furthermore, it is preferable to perform a purification step along with the heat treatment step of the group 5 transition metal compound. The purification step can be performed before or after the heat treatment of the group 5 transition metal compound, or it can be performed before the heat treatment and again after the heat treatment. The purification step can also be repeated one or more times. The purity of the group 5 transition metal-containing thin film formation precursor obtained by performing such a purification step can be increased.

[0043] Furthermore, the purification step can be carried out by using a method of vacuum distillation to remove the group 5 transition metal compound during the purification stage.

[0044] By performing heat treatment in this manner, or by carrying out heat treatment and purification processes, the iron (Fe) content of the present invention's high-purity Group 5 transition metal-containing thin film formation precursor may be significantly reduced.

[0045] When iron is present as an impurity, it can react with the amine group of the precursor compound to form a byproduct, which reduces the deposition efficiency of the Group 5 transition metal compound as a precursor. Since such iron has a similar volatility to the Group 5 transition metal-containing thin film formation precursor, there are limits to how much its content can be reduced through general purification methods such as distillation. Therefore, the application of a novel reduction technique like that of the present invention is preferable.

[0046] Furthermore, if iron is present as an impurity in a vanadium oxide thin film, the conductivity of iron can cause a change in the resistance of the thin film. This can alter the insulating properties, degrading the characteristics of the vanadium oxide thin film, which must have a high temperature coefficient of resistance and high resistance. Vanadium oxide has various oxidation states and crystallinity, and the temperature coefficient of resistance changes depending on the crystallinity. Therefore, in order to reproducibly obtain the desired thin film in the deposition process, a method must be proposed that allows for the production of high-purity precursors and the reduction of impurities.

[0047] The high-purity Group 5 transition metal-containing thin film formation precursor produced by the present invention may have an iron (Fe) content reduced by 40% or more compared to the aforementioned Group 5 transition metal compound. This value can be used as an indicator to confirm the purity of the Group 5 transition metal-containing thin film formation precursor.

[0048] To confirm the effectiveness of the manufacturing method of the present invention, a precursor for forming a Group 5 transition metal-containing thin film was manufactured as follows, and its physical properties were evaluated. (Tetrakisethylmethylamino)vanadium (V(EMA)4, TEMAV) was used as the target substance as the Group 5 transition metal compound, and the change in yield for each manufacturing method was evaluated.

[0049] Synthesis Example 1: Synthesis of (tetrakisethylmethylamino)vanadium V(EMA)4 Lithium-ethylmethylamine was prepared by slowly adding 85.27 g (1.44 mol) of ethylmethylamine dropwise to a flask containing 577 ml (1.44 mol) of a 2.5 M n-BuLi hexane solution in 1000 ml of n-hexane at -78°C. The solution was stirred at -78°C for 30 minutes, then raised to room temperature and stirred for a further 4 hours.

[0050] VOCl3-(THF) is reacted by slowly adding 0.288 mol (050 g) of VOCl3 dropwise to a flask containing 250 ml of THF (tetrahydrofuran) and 250 ml of n-hexane at -78°C. x The following was prepared: The solution was stirred at -78°C for 30 minutes, then heated to room temperature and stirred for a further 4 hours.

[0051] In a flask containing lithium-ethylmethylamine prepared in advance, VOCl3-(THF) synthesized at -78°C x The solution was slowly added dropwise and allowed to react. The solution was stirred at -78°C for 30 minutes, then stirred overnight at room temperature. The mixture was filtered, and the solvent and volatiles were evaporated under vacuum. The resulting dark green liquid was distilled at 70°C and 65 mTorr. The yield was 63 g (70%).

[0052] The obtained dark green liquid was subjected to a TGA measurement (using an SDT600 from TA Instruments) while increasing the temperature by 10°C / min under an atmosphere of nitrogen flow at 200 ml / min. The results are shown in Figure 1. As can be seen from the results in Figure 1, there was no residual mass, with a TGA of 0.0% measured at 10°C / min.

[0053] Furthermore, the heat flow of the obtained dark green liquid was measured using DSC (DSC25, TA Instrument Co., Ltd.) while increasing the temperature by 10°C / min under an atmosphere of nitrogen flowing at 50 ml / min. As shown in Figure 2, the thermal decomposition temperature was 266°C during the DSC analysis measured at 10°C / min.

[0054] Synthesis Example 2: Synthesis of (tetrakisethylmethylamino)vanadium V(EMA)4 Lithium-ethylmethylamine was prepared by slowly adding 85.27 g (1.44 mol) of ethylmethylamine dropwise to a flask containing 577 ml (1.44 mol) of a 2.5 M n-BuLi hexane solution in 1000 ml of n-hexane at -78°C. The solution was stirred at -78°C for 30 minutes, then raised to room temperature and stirred for a further 4 hours.

[0055] VOCl3-(DME) is reacted by slowly adding 0.00 g (0.288 mol) of VOCl3 dropwise to a flask containing 250 ml of DME (dimethoxyethane) and 250 ml of n-hexane at -78°C. x The following was prepared: The solution was stirred at -78°C for 30 minutes, then heated to room temperature and stirred for a further 4 hours.

[0056] The lithium-ethylmethylamine, prepared in advance, was slowly added dropwise to a flask at -78°C and reacted. The solution was stirred at -78°C for 30 minutes, then raised to room temperature and stirred overnight. The mixture was filtered, and the solvent and volatiles were evaporated under vacuum. The resulting dark green liquid was distilled at 70°C and 65 mTorr. The yield was 40.5 g (45%).

[0057] Comparative Example 1: Synthesis of (tetrakisethylmethylamino)vanadium V(EMA)4 Lithium-ethylmethylamine was prepared by slowly adding 85.27 g (1.44 mol) of ethylmethylamine dropwise to a flask containing 577 ml (1.44 mol) of a 2.5 M n-BuLi hexane solution in 1000 ml of n-hexane at -78°C. The solution was stirred at -78°C for 30 minutes, then raised to room temperature and stirred for a further 4 hours.

[0058] 350.00 g (0.288 mol) of VOCl was placed in a flask containing 1,000 ml of n-hexane and slowly added dropwise at -78°C to a flask containing lithium-ethylmethylamine prepared earlier. The solution was stirred at -78°C for 30 minutes, then raised to room temperature and stirred overnight. The mixture was filtered, and the solvent and volatiles were evaporated under vacuum to obtain a dark green liquid, which was then distilled at 70°C and 65 mTorr. The yield was 18 g (20%).

[0059] Comparing the manufacturing methods of Example 1, Example 2, and Comparative Example 1, the conventional manufacturing method in Comparative Example 1 had a yield of only 20%, while Examples 1 and 2 achieved yields of 70% and 45%, respectively, exceeding 40%. This represents yield improvements of 250% and 125%, respectively.

[0060] These results suggest that the improved manufacturing method of the present invention can produce Group 5 transition metal compounds suitable for use as precursors for forming Group 5 transition metal-containing thin films in high yield.

[0061] The Group 5 transition metal-containing thin film formation precursor obtained in high yield by applying the above manufacturing method can be easily purified by applying an appropriate heat treatment process. To confirm the efficiency of such a purification process, purification was performed under various heat treatment conditions as follows.

[0062] Example 1. Tests related to the effect of V(EMA)4 heat treatment on a mixture containing metal impurities. To verify the effectiveness of heat treatment in achieving high purity, V(EMA)4 samples containing various metal impurities as shown in Table 1 were prepared, and heat treatment effect-related tests were conducted according to Examples 1-1 to 1-10. The initial metal impurity values ​​were based on V(EMA)4 purified after synthesis. The test results from the examples are summarized in Table 1 below. (The heat treatment refers to the application of heat to the sample at the specified temperature for a predetermined time.) [Table 1]

[0063] Details for each of Examples 1-1 to 1-4 are as follows.

[0064] Example 1-1. Comparative test of the effect of V(EMA)4 heat treatment on a mixture containing metal impurities after purification (Fe 708 ppb) Equal amounts of V(EMA)4 containing 708 ppb of Fe were separated to form two samples, Sample 1 and Sample 2. Sample 1 was heat-treated at 140°C for 2 hours, and Sample 2 was heat-treated at 140°C for 12 hours. To confirm the effect of heat treatment time at the same heat treatment temperature for each sample, distillation was performed at 70°C and 65 mTorr to obtain the compound in liquid form. From these results, it was confirmed that the sample that underwent a longer heat treatment time at the same heat treatment temperature after purification showed a greater reduction in Fe metal content compared to the sample that underwent a shorter heat treatment time.

[0065] Furthermore, the second sample obtained was measured using an inductively coupled plasma mass spectrometer (ICP-MS, Perkinelmer Nexion 300s). The results are shown in Figure 3.

[0066] Examples 1-2. Comparative test of the effect of V(EMA)4 heat treatment on a mixture containing metal impurities after purification (Fe 1130 ppb) Samples 3, 4, 5, and 6 were taken from V(EMA)4 containing 1,130 ppb of Fe, using equal amounts. Sample 3 was heat-treated at 140°C for 2 hours, sample 4 at 140°C for 4 hours, sample 5 at 140°C for 8 hours, and sample 6 at 140°C for 12 hours. To confirm the effect of heat treatment time at the same heat treatment temperature for each sample, distillation was performed at 70°C and 65 mTorr to obtain the compounds in liquid form. From these results, it was confirmed that after purification, samples that were heat-treated for a longer period at the same heat treatment temperature showed a tendency to reduce Fe metal content compared to samples that were heat-treated for a shorter period.

[0067] Examples 1-3. Comparative test of the effect of V(EMA)4 heat treatment on a mixture containing metal impurities after purification (Fe 513 ppb) Samples 7 and 8 were taken in equal amounts from V(EMA)4 containing 513 ppb of Fe. Sample 7 was heat-treated at 140°C for 12 hours, while sample 8 was not heat-treated. Each sample was distilled at 70°C and 65 mTorr to obtain the compound in liquid form. From these results, it was confirmed that the heat-treated sample showed a greater reduction in Fe metal content compared to the untreated sample.

[0068] Example 1-4. Comparative test of heat treatment effects by purification order using V(EMA)4 (Fe 1209 ppb) Sample 9 was taken from V(EMA)4, which was obtained containing 1209 ppb of Fe. Sample 9 was subjected to primary heat treatment at 140°C for 12 hours. After distillation of this sample at 70°C and 65 mTorr to obtain a liquid compound, sample 10 was taken. Sample 10 was subjected to secondary heat treatment at 140°C for 12 hours. This sample was distilled at 70°C and 65 mTorr to obtain a liquid compound. From these results, it was confirmed that the sample subjected to two heat treatments showed a greater reduction in Fe metal content compared to the sample subjected to one heat treatment.

[0069] Although the present invention has been described with reference to preferred embodiments as described above, it is not limited to these embodiments, and various modifications and alterations can be made by persons with ordinary skill in the art to which the invention pertains without departing from the spirit of the invention. Such modifications and alterations should be understood to be within the scope of the present invention and the appended claims.

Claims

1. The steps include: reacting a group 5 transition metal supplier and a solvent to form a complex compound; A method for producing a high-yield Group 5 transition metal-containing thin film precursor, comprising the step of reacting the complex compound with a ligand or ligand salt to form a Group 5 transition metal compound.

2. The method for producing a high-yield Group 5 transition metal-containing thin film precursor according to claim 1, characterized in that the solvent is selected from compounds containing lone pairs of electrons.

3. The method for producing a high-yield Group 5 transition metal-containing thin film formation precursor according to claim 1, characterized in that the solvent is a compound containing either a nitrogen atom (N) or an oxygen atom (O), or both thereof.

4. The method for producing a high-yield Group 5 transition metal-containing thin film formation precursor according to claim 1, characterized in that the solvent is any of tetrahydrofuran (THF), dimethoxyethane (DME), diethyl ether, dimethoxymethane (DMM), 1,4-dioxane, pyridine, 2,2'-bipyridine, acetonitrile, tetramethylethylenediamine, or a mixture thereof.

5. The method for producing a high-yield Group 5 transition metal-containing thin film precursor according to claim 1, characterized in that the step of forming the Group 5 transition metal compound is to react the complex compound with a ligand or ligand salt in the presence of at least one solvent selected from a polar solvent and a nonpolar solvent.

6. The method for producing a high-yield Group 5 transition metal-containing thin film formation precursor according to claim 1, characterized in that the yield of the Group 5 transition metal compound obtained by the step of forming the Group 5 transition metal compound is 40% or more.

7. A method for producing a high-yield Group 5 transition metal-containing thin film formation precursor according to claim 1, characterized in that the yield improvement rate of the Group 5 transition metal compound obtained by the step of forming the Group 5 transition metal compound is 100% or more.

8. The step further includes heat-treating the group 5 transition metal compound obtained by the step of forming the group 5 transition metal compound at a heat treatment temperature, The method for producing a high-yield Group 5 transition metal-containing thin film formation precursor according to claim 1, characterized in that the heat treatment step is performed at a heat treatment temperature of 80 to 240°C for 0.01 to 48 hours.

9. The method for producing a high-yield Group 5 transition metal-containing thin film formation precursor according to claim 8, characterized in that the heat treatment step involves raising the temperature from room temperature to the heat treatment temperature at a heating rate of 0.1 to 10°C / min, and then performing the heat treatment.

10. The method for producing a high-yield Group 5 transition metal-containing thin film formation precursor according to claim 8, characterized by comprising the step of purifying the Group 5 transition metal compound at least once before or after heat treatment of the Group 5 transition metal compound.

11. The method for producing a high-yield Group 5 transition metal-containing thin film formation precursor according to claim 10, characterized in that the purification step involves purifying the Group 5 transition metal compound by vacuum distillation.

12. The method for producing a high-yield Group 5 transition metal-containing thin film formation precursor according to claim 8, wherein the heat treatment step is characterized by i) heat treatment in a container on which the Group 5 transition metal compound is supported, ii) heat treatment of the Group 5 transition metal compound in a transfer section where it is moved from the container to another container, or iii) heat treatment of the Group 5 transition metal compound in a container on which the Group 5 transition metal compound is supported and in a transfer section where it is moved from the container to another container.

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