Low pressure process for synthesis of pt(PF3)4 involving a soluble intermediate and storage of obtained pt(PF3)4
Patent Information
- Application Number
- TW113147915
- Authority / Receiving Office
- TW · TW
- Patent Type
- Patents
- Current Assignee / Owner
- Priority Date
- 2021-12-09
- Filing Date
- 2022-12-05
- Publication Date
- 2026-10-11
- Estimated Expiration
- 2042-12-04
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Figure TWG2TB001915262_001 
Figure TWG2TB001915262_002 
Figure TWG2TB001915262_003
Abstract
Description
Low-pressure method for the synthesis of Pt(PF3)4 involving soluble intermediates and storage of the obtained Pt(PF3)4 The present invention relates to a Pt(PF) film-forming composition used as a precursor. 3) Synthesis and storage of 4. Pt(PF 3) 4 is selected from Pt(Hal) 2 (Hal = F, Cl, Br or I) or Pt(Hal) 2(PF 3) x (Hal = F, Cl, Br or I; x = 1, 2) platinum compounds, metal powders and PF 3. Able to dissolve Pt(Hal) at low pressure 2(PF 3) x (reaction intermediate) was synthesized in anhydrous solvent, where Pt(Hal) 2(PF 3) x Can be made of Pt(Hal) 2 and PF 3 is formed. Then the obtained Pt(PF 3) Store at room temperature in the absence of air and moisture in devices and ampoules made of metal such as stainless steel and preferably with passivated or electropolished interior surfaces. Chemical vapor deposition (CVD) and atomic layer deposition (ALD) methods are gaining significant attention for the production of catalysts and batteries on an industrial scale. Suitable precursors for high-throughput industrial processes ideally should have high vapor pressures at room temperature to ensure maximum utilization in the shortest possible time and at temperatures that do not compromise the precursor's stability. Platinum is widely used as a catalyst, and a variety of materials containing platinum on a support are available. However, due to the lack of suitable platinum precursors, the application of platinum deposition methods from the vapor phase is rare. For example, platinum hexafluoride (PtF 6, CAS # 13693-05-5), is a solid at room temperature and, although volatile at room temperature, is rarely used as a deposition precursor due to its very strong oxidizing properties and correspondingly very strong etching characteristics. Deposition methods widely cited (MeCp)PtMe 3 (CAS # 94442-22-5) has a vapor pressure of 1 Torr at 69°C but begins to gradually decompose at 50°C (Journal of Vacuum Science & Technology, B: Microelectronics and Nanometer Structures (1990), 8(6), 1826-9), precluding the use of the given compound for high-volume delivery methods. Complex Pt(PF 3) 4 (CAS # 19529-53-4) is a volatile liquid at room temperature with a vapor pressure of 36 Torr (RD Sanner et al., Report (1989), (UCRL-53937; Serial No. DE90000902)), making it an almost ideal potential precursor for Pt deposition from the vapor phase. However, this compound has very limited commercial availability. The reason for its unscalability may be its close proximity to Pt(PF). 3) The technical difficulties associated with the synthesis of 4, an almost ideal potential precursor for the deposition of Pt from the vapor phase. However, this compound has very limited commercial availability (only from one supplier in Japan [Japan Advanced Chemicals], on a gram scale), and no suitable ALD process using this chemical has been reported to date. The reason for the non-scalability may be related to the difficulty in synthesizing Pt (PF) at the gram scale level and even more difficult to scale up industrially with acceptable yields and practical operating conditions. 3) 4. Related technical difficulties. By reaction (1) at 100-150 atm. PF The yield of Pt(PF) was 70%-80% at 3 and 100°C using fine, oxide-free copper powder on a gram scale. 3) The initial synthesis of 4 (Angew. Chem. Int. Ed. [German Applied Chemistry] 1965, 4, 521). The synthesis formula is only a sentence in the reference, and the subsequent references use the same method without any details about the reaction and equipment. The reaction requires PF to be heated under high pressure. 3 gases are applied to two solids (PtCl 2 and Cu powder) and is almost unscalable for chemists skilled in the art. PtCl 2+ 2Cu + PF 3(excess) → Pt(PF 3) 4+ 2CuCl (1) It is worth noting that PtCl 2 and PF Reaction of 3 (2) at 60-80°C and under an undisclosed pressure afforded Pt(PF) in only 1% yield. 3) 4 (Inorg. Nucl. Chem. Letters, Vol. 4, pp. 275-278, 1968). This low yield makes the process impossible to implement for industrial applications. 2+ PF 3(excess) → Pt(PF 3) 4+ Other products (2) Flow reactions (3) from the same starting compounds at undisclosed pressures yielded only donor-acceptor adducts (Inorg. Nucl. Chem. Letters, Vol. 4, pp. 275-278, 1968). 3PtCl 2+ PF 3 (excess) → PtCl 2(PF 3) 2+ [PtCl 2(PF 3)] 2(3) Compound PtCl 2(PF 3) 2 and [PtCl 2(PF 3)] 2 by solid PtCl 2 and PF 3 Gas Synthesis (J. Chatt, AA Williams, J. Chem. Soc. [Journal of the American Chemical Society] [London] 1951, 3061). According to a sentence on page 200 of Zeitschrift fur Anorganische und Allgemeine Chemie [Journal of Organic and Inorganic Chemistry], vol. 364 (Band), 1969, pp. 192-208, solid compounds can be reacted with PF at undisclosed "higher" pressures. 3 reaction to form Pt(PF 3) 4. It can be assumed that the "higher pressure" is 40-150 atm, since this range was reported in Zeitschrift fur Anorganische und Allgemeine Chemie [Journal of Organic and Inorganic Chemistry], Vol. 364, 1969, pp. 192-208 for the synthesis of Pt(PF 3) 4. Compound PtCl 2(PF 3) 2Soluble in polar solvent CDCl 3, and its NMR was reported by J. Chem. Res., Syn. [Chemical Research Journal, Summary], 1981, 2, 38. According to J. Chem. Soc. [Journal of the American Chemical Society] [London] 1951, 3061, PtCl 2(PF 3) 2 has a low solubility in benzene and a molar concentration of 0.005 - 0.01 M, and PtCl 2(PF 3) The melting point of 2 is 118.3°C. 2(PF 3) The FTIR spectrum of 2 was disclosed in Journal of Chemical Research, Synopses (1981), (2), 37. Alternatively, Pt(PF 3) 4 was prepared on a gram scale in a rotary autoclave which is difficult to obtain by reacting (4) at 40 atm PF 3 in 95% yield (Zeitschrift fur Anorganische und Allgemeine Chemie [Journal of Organic and Inorganic Chemistry]. Vol. 364. 1969, 192-208). 4+ 4Cu + 4PF 3→ Pt(PF 3) 4+ 4CuCl (4) PtCl 4+ 6PF 3→ Pt(PF 3) 4+ 2PF 3Cl 2(5) It is noteworthy that there is no copper reaction (5) to produce PF 3Cl 2. Due to its considerable volatility, Pt(PF 3) 4 complicates the purification of PF (Zeitschrift fur Anorganische und Allgemeine Chemie [Journal of Organic and Inorganic Chemistry]. Vol. 364. 1969, 192-208). Although the addition of copper reduces the 3Cl 2, but this means that reactions (4) and (5) can provide impure Pt(PF 3) 4, which does not meet the quality standards of CVD and ALD precursors. Notably, reaction (4) also requires mixing the two solids and mixing them with PF 3 Gas contact, causing the scalability issues already mentioned. PtCl 4 and excessive PF A reaction of 3 makes scaling up even less realistic. RU 2478576 C2 revealed PF at 2-6.3 MPa (19.7-62.2 atm) 3 two-step method (6a and 6b), in which K 2PtCl 6 and PF 3. CuO was reduced in the same autoclave as before. CuO + H 2→ Cu + H 2O (6a) K 2PtCl 6+ 4Cu+ PF 3(excess) → Pt(PF 3) 4+ 4CuCl + 2KCl (6b) RU 2201463 C1, US 7044995 B2, Terekhov et al. (Terekhov et al., International Symposium on Recycling of Metals and Engineered Materials, Proceedings, 4th, October 22-25, 2000, pp. 487-491) and Kovtun et al. (Publications of the Australasian Institute of Mining and Metallurgy (2002), 2 / 2002, 367-372) disclose the use of "PGM cobalt" or "raw materials" with PF 3 The interaction of gases forms volatile Pt(PF 3) 4 and extract platinum from ore. Assuming that the raw material contains Pt metal and is reacted with PF by (7d) 3 interactions. However, as first reported in 1891 (H. Moissan, Bull. Soc. Chim. France [Bulletin of the French Chemical Society] 5, 454 (1891)), Pt and PF 3 Provide platinum compound F 5PPt and the compound is considered to be similar to (PCl 3) PtCl 2. 3Pt + 4HNO 3+ 18HCl → 3H 2PtCl 6+ 4NO + 8H 2O (7a) H 2PtCl 6+ 2NH 3→ (NH 4) 2PtCl 6(7b) (NH 4) 2PtCl 6+ H 2 = 2NH 4Cl + 4HCl + Pt (under ultrasonic irradiation) (7c) Pt + PF 3(excess) → Pt(PF 3) 4(7d) In addition, according to Chem. Ber. [German Chemical Journal] 101, 138 -142 (1968), Pt metal does not react with PF under any conditions. 3 reaction. US 7044995 B2 discloses that finely dispersed Pt metal (platinum black, particle size < 20 μm) does not react with PF 3 reaction, and only the "activated" Pt metal obtained by the multi-step process (7a-7c) and the reduction with hydrogen under ultrasonic irradiation in step (7c) can react with PF 3 reactions. Solvent effects on the 2 The reaction may be negative, since according to Zhurnal Neorganicheskoi Khimii [Russian Journal of Inorganic Chemistry] (1970), 15(9), 2445-8, with PtCl 2+ I 2 = PtCl 2I Compared with the pure reaction of 2, the reaction of these reagents in organic solvents gave various products, but no PtCl 2I 2. Several types of solvents and PF 3. PtCl 2 reacts with the reduced Pt species and therefore cannot be used to synthesize Pt(PF 3) 4. This class of solvents includes primary amines because they react with PF 3 reactions produce RNHPF 2. (RNH) 2PF 2H and (RNH) 2PF (see J. Chem. Soc. A (1970), (11), 1935-8). Tertiary amines, such as NMe 3. NEt 3 and PF 3 forms adducts (see Inorganic Chemistry (1963), 2, 384-8). Alcohols and PF 3 to form organophosphites (see Transactions of the Illinois State Academy of Science (1936), 29 (No. 2), 89-91). P(Hal) General pattern of reactivity of 3 (Hal = Cl, Br) towards alcohols. Dienes, alkenes, unsaturated aldehydes, ketones and PF 3 reaction to form addition compounds, such as for PCl 3 and PBr 3 (see Uspekhi Khimii [Russian Chemical Review] (1968), 37(5), 745-77). 3 reacts with Pt(II) compounds (see Zhurnal Obshchei Khimii [Russian Journal of General Chemistry] (1975), 45(3), 512-18; Inorganica Chimica Acta [Inorganic Chemistry Acta] (1997), 264(1-2), 297-303). Halogenated hydrocarbons can react with Pt compounds via oxidative addition under the reaction conditions, as described in Organometallics [Organometallics] (2019), 38(10), 2273; Organometallics [Organometallics] 2009. , The oxidative addition of alkyl and aryl halides to platinum complexes is a well-documented reaction, as shown in selected examples in Organometallics (1987), 6(12), 2548. In summary, for Pt(PF 3) The existing synthesis methods of 4 are strongly dependent on the reaction conditions, and changes in the conditions can significantly reduce the Pt(PF 3) The yields of 4 or different products were provided, indicating that the method lacks robustness and that the claimed PF as claimed in RU 2478576 C2 has not been reported so far. 3 Synthesis methods with pressures below 3 MPa (29.6 atm, 420 psig). Most syntheses require specialized equipment or conditions, such as high-pressure autoclaves, that are not typically available for scaling up the methods to large scale. In particular, existing methods lack technical details, and Pt(PF) has not been reported in any references. 3) Furthermore, all disclosed methods are essentially dry processes, which also poses a significant challenge in scaling up to industrial scale. There are many references to the catalytic conversion of hydrocarbons by platinum compounds, such as, Journal of the American Chemical Society (2002), 124(42), 12550-12556. The catalytic activity of Pt compounds was studied for the model system Pt in Jackson et al., J. Am. Chem. Soc. 1997, 119, 7567-7572. 4(PF 3) 8- saturated and aromatic cyclic hydrocarbons are described. 4(PF 3) 8 The small platinum clusters produced react with a variety of saturated and aromatic cyclic hydrocarbons (cyclohexane, benzene, toluene). Jackson et al. demonstrated the catalytic and dehydrogenation behavior of platinum. Therefore, it can be assumed that the introduction of a hydrocarbon solvent into the reaction system followed by heating will result in a mixture of products due to the various catalytic reactions, and this can be considered to be a good strategy for Pt(PF) 3) The selective synthesis of 4 is disadvantageous. 3) 4 was never synthesized and manipulated in organic solvents, and only anhydrous HF and SO were used. 2 as a solvent to study Pt(PF 3) 4 Chemistry (Drews et al., Chem. Eur. J. 2008, 14, 4280 - 4286). Provides a method for scalable production of Pt(PF) with high yield 3) The method of 4 would be a significant advance, because to date, the potential ideal Pt(PF 3) 4 Precursors have not been applied simply due to the lack of scalable methods. A method for synthesizing Pt(PF 3) 4 (CAS # 19529-53-4), which comprises the following steps: 2(PF 3) x The platinum compound is dissolved in an anhydrous solvent to form Pt(Hal) 2(PF 3) x Solution, where Hal = F, Cl, Br or I, x = 1, 2; Mix metal powder and excess PF 3 added to the Pt(Hal) 2(PF 3) x solution; and under reaction conditions by Pt(Hal) 2(PF 3) x PF 3 reacts with the metal powder to form Pt(PF 3) 4. The disclosed method may include one or more of the following aspects: • Reaction conditions include a reaction temperature ranging from about -120°C to 200°C; • Reaction conditions include a reaction temperature ranging from about 30°C to 200°C; • Reaction conditions include a reaction temperature ranging from room temperature to about 180°C; • Reaction conditions include a reaction temperature ranging from room temperature to about 130°C; • Reaction conditions include a reaction temperature ranging from about 80°C to 130°C; • Reaction conditions include a reaction pressure ranging from about 10 psig to about 3000 psig; • Reaction conditions include a reaction pressure ranging from about 20 psig to about 1000 psig; • Reaction conditions include a reaction pressure ranging from about 20 to about 300 psig; • Reaction conditions include a reaction pressure less than about 300 psig; • The anhydrous solvent has a boiling point greater than 150°C; • The anhydrous solvent has a boiling point greater than 200°C; • The metal powder is copper, zinc or aluminum powder; • The metal powder is copper powder; • The metal powder is zinc powder; • The metal powder is aluminum powder; • The metal powder has an electrode potential lower than that of Pt; • Under the reaction conditions, the metal powder does not react with PF 3 interacts with and does not interact with PF 3 to form a complex; • the metal powder has a suitable particle size range that allows it to remain in powder form during the reaction process; • the metal powder has a particle size ranging from 200-900 microns; • the metal powder has a particle size ranging from 300-500 microns; • further comprising the steps of synthesizing the platinum compound Pt(Hal) 2(PF 3) x (Hal = F, Cl, Br or I; x = 1, 2), which comprises the following steps: Replacing a compound having the general formula Pt(Hal) 2 platinum precursor is dispersed into the anhydrous solvent to form Pt(Hal) 2 suspension, wherein Hal = F, Cl, Br or I; PF 3Introduction of the Pt(Hal) 2 in suspension; and by PF 3 and Pt(Hal) 2 reaction to form a platinum compound Pt(Hal) 2(PF 3) x(Hal = F, Cl, Br or I; x = 1, 2) in an anhydrous solvent; • Platinum precursor Pt(Hal) 2 series anhydrous; • platinum precursor Pt(Hal) 2-series PtCl 2; • Platinum precursor Pt(Hal) 2-series anhydrous PtCl 2; • Platinum compound Pt(Hal) 2(PF 3) x (Hal = F, Cl, Br or I, x = 1, 2) is anhydrous; • Platinum compound Pt(Hal) 2(PF 3) x (Hal = F, Cl, Br or I, x = 1, 2) is PtCl 2(PF 3) 2; • Platinum compound Pt(Hal) 2(PF 3) x (Hal = F, Cl, Br or I, x = 1, 2) is anhydrous PtCl 2(PF 3) 2; • further comprising the following steps: purifying Pt(PF) in a metal trap in the absence of air and moisture 3) 4; and the purified Pt(PF 3) 4 is stored in a container made of metal, wherein the step of storing comprises the steps of removing moisture from the inner surface of the container; and electropolishing the inner surface of the container, or introducing purified Pt (PF 3) 4 Use PF before 3 passivation container; • The metal used for the trap is selected from carbon steel, stainless steel, or stainless steel 316 alloy; • The metal used for the container is selected from carbon steel, stainless steel, or stainless steel 316 alloy; • The anhydrous solvent is a hydrocarbon solvent; • The hydrocarbon solvent is selected from a general formula (C n H 2n+1 ) 2O (n ≥ 1) and H 3C(O(CH 2) 2) n OCH 3 (n ≥ 1) oxyhydrocarbon solvents; • hydrocarbon solvents are selected from the group consisting of n H 2n+1 ) x C 6H 6-x (x ≥ 1, n ≥ 1) aromatic hydrocarbon solvents; • hydrocarbon solvents are selected from the group consisting of n H 2n+2 (n ≥ 1) alkane solvent; • The anhydrous solvent is a dry alkane solvent selected from decane, dodecane, tridecane, tetradecane, pentadecane and hexadecane; • The anhydrous solvent is a dry aromatic solvent selected from xylene, mesitylene, cymene, pentylbenzene, diisopropylbenzene, diisobutylbenzene, etc.; • The anhydrous solvent is a dry ether solvent selected from dibutyl ether, dihexyl ether, dioctyl ether, diethylene glycol dimethyl ether, triethylene glycol dimethyl ether, tetraethylene glycol dimethyl ether, etc.; • The anhydrous solvent is an aromatic solvent selected from xylene, mesitylene, cymene, pentylbenzene, diisopropylbenzene, diisobutylbenzene, etc.; • The dry ether solvent is preferably dibutyl ether, dihexyl ether, dioctyl ether, triethylene glycol dimethyl ether, tetraethylene glycol dimethyl ether; • Preferred dry aromatic solvents are xylene, mesitylene, cymene, pentylbenzene, diisopropylbenzene, and diisobutylbenzene. • Preferred dry alkane solvents are dodecane, tridecane, tetradecane, pentadecane, hexadecane, and a mixture of alkanes known as mineral oil. • Anhydrous solvents are capable of dissolving the reaction intermediates. • Anhydrous solvents are capable of dissolving Pt(Hal). 2(PF 3) x (Hal = F, Cl, Br or I, x = 1, 2); • Anhydrous solvents can dissolve PtCl 2(PF 3) 2; • Anhydrous solvents do not react with Pt(PF 3) 4 reaction; • Anhydrous solvents do not react with Pt(Hal) 2 (Hal = F, Cl, Br or I); • Anhydrous solvents do not react with PtCl 2 reaction; • Anhydrous solvent is xylene; • Anhydrous solvent is hexadecane; • Pt(PF 3) The yield of 4 is in the range of about 70%-99.9%; • Pt(PF 3) The yield of 4 is in the range of about 70%-95%; • Pt(PF 3) The yield of 4 is in the range of about 70%-93%; • Pt(PF 3) 4 has a purity greater than 99% by weight; • Pt(PF 3) 4 has a purity greater than 99.5% by weight; • Pt(PF 3) 4 has a purity of approximately 90%-99.9% by weight; • Pt(PF 3) 4 has a purity of approximately 99.0%-99.9% by weight; • Pt(PF 3) 4 has a purity of about 99.5% to 99.9% by weight; and • the Pt(PF 3) 4. Scalable to large industrial scale. Also disclosed is a method for producing and storing Pt(PF 3) 4 (CAS # 19529-53-4), the method comprising the following steps: a) forming a platinum precursor Pt(Hal) 2 (where Hal = F, Cl, Br or I) and a suspension of metal powder in an anhydrous solvent; b) excess PF 3Introduction of Pt(Hal) 2 and the metal powder in the suspension; c) under low pressure conditions, by PF 3 and Pt(Hal) The reaction of 2 forms a soluble reaction intermediate Pt(Hal) in anhydrous solvent 2(PF 3) x (wherein Hal = F, Cl, Br or I; x = 1, 2); d) in the anhydrous solvent by Pt (Hal) 2(PF 3) x 、The metal powder and PF 3 to form Pt(PF 3) 4; e) Purification of Pt(PF) in a metal trap in the absence of air and moisture 3) 4; and f) the purified Pt(PF 3) 4 is stored in a container made of the metal. The disclosed method may include one or more of the following aspects: • Platinum precursor Pt(Hal) 2-series PtCl 2; • the anhydrous solvent has a boiling point higher than 150°C; • the anhydrous solvent has a boiling point higher than 200°C; • the anhydrous solvent is selected from the following hydrocarbon solvents: n H 2n+1 ) 2O (n ≥ 1) and H 3C(O(CH 2) 2) n OCH 3 (n ≥ 1) oxygenated hydrocarbon solvent, having the general formula (C n H 2n+1 ) x C 6H 6-x (x ≥ 1, n ≥ 1) aromatic solvent or a solvent having the general formula C n H 2n+2 (n ≥ 1) alkane solvents; • anhydrous solvents are xylene or hexadecane; •Anhydrous solvents are able to dissolve reaction intermediates; •Anhydrous solvents can dissolve Pt(Hal) 2(PF 3) x (Hal = F, Cl, Br or I, x = 1, 2); • Anhydrous solvents capable of dissolving PtCl 2(PF 3) 2; •Anhydrous solvents do not react with Pt(PF 3) 4 reactions; •Anhydrous solvents do not react with Pt(Hal) 2 (Hal = F, Cl, Br or I) reaction; • Anhydrous solvents do not react with PtCl 2 reaction; • the reaction temperature ranges from about 30°C-200°C; • the reaction temperature ranges from about 80°C-130°C; • the low pressure condition is a pressure less than about 300 psig; • the low pressure condition is a pressure ranging from about 20 to 300 psig; • the metal powder is copper, zinc or aluminum powder; • the metal powder is copper powder; • the metal powder has an electrode potential lower than the electrode potential of Pt; • under the reaction conditions, the metal powder does not react with PF 3 interacts with and does not interact with PF 3 to form a complex; • the metal powder has a suitable particle size range that allows it to remain in powder form during the reaction process; • the metal powder has a particle size ranging from 200-900 microns; • the metal powder has a particle size ranging from 300-500 microns; • Pt(PF 3) The yield of 4 ranged from approximately 70% to 99.9%; •Pt(PF 3) The yield of 4 was in the range of approximately 70%-95%; •Pt(PF 3) The yield of 4 was in the range of about 70%-93%; • After purification, Pt(PF 3) The purity of 4 is about 90 wt.%-99.9 wt.%; • After purification, Pt(PF 3) 4 has a purity of 99.0 wt.%-99.9 wt.%; • the metal for the well and the metal for the container are selected from carbon steel, stainless steel, or stainless steel 316 alloy; and • further comprising the steps of: electropolishing the inner surface of the container, or introducing purified Pt(PF 3) 4 Use PF before 3. Passivation container. Also disclosed is a method for producing and storing Pt(PF 3) 4 (CAS # 19529-53-4), the method comprising the following steps: a) forming a platinum precursor Pt(Cl) 2 in a suspension in an anhydrous solvent selected from xylene or hexadecane; b) excess PF 3Introduction of Pt(Cl) 2 in a suspension by PF 3 and Pt(Cl) The reaction of 2 forms Pt(Cl) 2(PF 3) x (x = 1, 2) solution in an anhydrous solvent; c) adding copper powder to the Pt(Cl) 2(PF 3) x (x = 1, 2) solution; d) at reaction temperatures ranging from 30°C-200°C and reduced PF ranging from 20 to 300 psig 3. Under pressure, copper powder, PF 3 and Pt(Cl) 2(PF 3) x The reaction between them forms Pt(PF 3) 4; e) Purification of Pt(PF) in a stainless steel trap in the absence of air and moisture 3) 4; and f) the purified Pt(PF 3) 4 is stored in a container made of stainless steel under the condition of being free of air and moisture, wherein the inner surface of the container is electropolished or treated with PF 3. Passivation. The disclosed method may include one or more of the following aspects: • the copper powder has a particle size ranging from 200-900 microns; and • the copper powder has a particle size ranging from 300-500 microns. Symbols and nomenclature The following detailed description and claims utilize many abbreviations, symbols, and terms that are commonly known in the art. Although definitions are typically provided with the first instance of each acronym, such as stainless steel (SS), certain abbreviations, symbols, and terms are used throughout the following description and claims and include the following. The following detailed description and claims utilize a number of abbreviations, symbols, and terms that are commonly known in the art. As used herein, the indefinite article "a" or "an" means one or more than one. As used herein, "about" or "around" or "approximately" in the text or claims means ±10% of the stated value. As used herein, "room temperature" in the text or claims means from about 18°C to about 25°C. As used herein, "atmospheric pressure" in the text or claims means approximately 1 atm. Standard abbreviations for the elements of the Periodic Table are used herein. It should be understood that an element may be referred to by these abbreviations (e.g., Si refers to silicon, N refers to nitrogen, O refers to oxygen, C refers to carbon, H refers to hydrogen, and Hal refers to halogen (e.g., F, Cl, Br, I)). Unique CAS Registry Numbers (ie, "CAS") assigned by the Chemical Abstract Service are provided to identify specific molecules disclosed. As used herein, the term "hydrocarbon" refers to a saturated or unsaturated functional group containing only carbon and hydrogen atoms. As used herein, the term "low pressure", "low reaction pressure" or "low PF" 3 pressure” means a pressure below 300 psig or below 20 atm. The same applies to “reduced pressure”, which means reducing or lowering the pressure to below 300 psig or 20 atm. In some cases, “low pressure”, “low reaction pressure” or “low PF "3 pressure" may refer to a pressure range from 20 psig to 300 psig. Ranges may be expressed herein as from about one particular value and / or to about another particular value. When such a range is expressed, it is understood that another embodiment is from one particular value and / or to the other particular value, as well as all combinations within the stated range. Any and all ranges described herein include their endpoints (i.e., x = 1 to 4 or x ranges from 1 to 4 including x = 1, x = 4, and x = any value therebetween), regardless of whether the term "inclusive" is used. References herein to "one embodiment" or "an embodiment" mean that a particular feature, structure, or characteristic described in connection with that embodiment may be included in at least one embodiment of the present invention. The phrase "in one embodiment" appearing in various places in the specification does not necessarily refer to the same embodiment, nor are separate or alternative embodiments necessarily mutually exclusive of other embodiments. This also applies to the term "implementation." As used herein, the word "exemplary" is used herein to mean serving as an example, instance, or illustration. Any aspect or design described herein as "exemplary" is not necessarily to be construed as preferred or advantageous over other aspects or designs. Instead, the use of the word exemplary is intended to describe concepts in a concrete manner. Additionally, the term "or" is intended to mean an inclusive "or" rather than an exclusive "or." That is, unless specified otherwise or clear from the context, "X employs A or B" is intended to mean any of the natural inclusive permutations. That is, if X employs A; X employs B; or X employs both A and B, then "X employs A or B" is satisfied in any of the foregoing instances. Furthermore, the articles "a" and "an," as used in this application and the appended claims, should generally be construed to mean "one, one, or more," unless specified otherwise or clear from the context to indicate a singular form. Disclosed are methods for synthesizing, producing, manufacturing and storing Pt(PF 3) 4 (CAS # 19529-53-4). The disclosed method can be scaled up to produce Pt(PF 3) 4, and the produced Pt(PF 3) 4 can be used as a precursor for the deposition of Pt-containing films in microelectronic devices or in the catalyst industry. The disclosed synthesis method can be to use an insoluble platinum compound Pt(Hal) 2 (Hal = F, Cl, Br or I) and a soluble reaction intermediate platinum compound Pt(Hal) 2(PF 3) x (Hal = F, Cl, Br or I; x = 1, 2) Pt(PF 3) 4 was synthesized by a two-step wet method, which involved the reaction of insoluble Pt(Hal) 2 (Hal = F, Cl, Br or I) suspension to form a soluble reaction intermediate, and the soluble intermediate reacts with metal powder and co-reactant such as PF 3 reaction to form Pt(PF 3) 4. Alternatively, due to the soluble intermediate Pt(Hal) 2(PF 3) x (Hal = F, Cl, Br or I; x = 1, 2) can be separated and purified, so the disclosed synthesis method can be Pt(PF 3) 4 was synthesized in a one-step wet process using soluble Pt(Hal) 2(PF 3) x (Hal = F, Cl, Br or I; x = 1, 2) with metal powder and co-reactants such as PF 3 reacts under certain reaction conditions to form Pt(PF 3) 4. Preferably, Hal = Cl. Preferably, the metal powder is copper powder. Furthermore, it is disclosed that Pt(PF 3) A robust, high-yield, and scalable synthesis of 4 that can be performed at low pressure and in common reactors or apparatuses is provided. More specifically, Pt(PF 3) 4 can be selected from Pt(Hal) 2 (Hal = F, Cl, Br or I) or Pt(Hal) 2(PF 3) x Platinum compounds (Hal = F, Cl, Br or I; x = 1, 2) and PF 3 and metal powders such as copper powder, in low PF 3 pressure in an anhydrous solvent. The metal powder may have a particle size ranging from about 200-900 microns, preferably from about 300-500 microns. The anhydrous solvent may be capable of dissolving Pt(Hal) 2(PF 3) x (Hal = F, Cl, Br or I; x = 1, 2) (reaction intermediate), where Pt(Hal) 2(PF 3) x (Hal = F, Cl, Br or I; x = 1, 2) can be synthesized from Pt(Hal) under certain reaction conditions, such as low pressure. 2 and PF 3 is formed. In this article, the platinum compound Pt(Hal) 2(PF 3) x (Hal = F, Cl, Br or I; x = 1, 2) can be isolated and purified for use in the synthesis of Pt(PF 3) 4 reactants or starting materials. Pt(PF) 3) The yield of 4 can be in the range of about 70%-99.9%. The present disclosure also includes the product Pt (PF 3) 4 purification method and purified Pt(PF 3) 4 Storage conditions in the container. Pt(PF 3) 4 Store in air- and moisture-free containers and ampoules made of stainless steel, preferably with passivated or electropolished inner surfaces. 3) 4 Storage at room temperature in metal containers without changing its purity, such as stainless steel containers and stainless steel containers with passivated or electropolished inner surfaces. As described above, the absence of scalable methods in the art may be because commonly available reactors for pilot plant synthesis and large-scale manufacturing are not designed to operate at high pressures and are not designed for effective stirring (mixing) of air-sensitive solids. That is, commercially available reactors (e.g., from High Pressure Equipment Company) capable of operating at high pressures of about 100 atm do not have the stirring capability necessary for the reaction to proceed. In addition, commercially available reactors (e.g., from Buchiglas USA) are difficult to cool to a temperature sufficient to condense the PF in the reactor. 3 even dry ice temperature is required. The use of specially designed stirring shafts can improve the stirring of solids to some extent, but will not solve the problem of platinum metal and the reduction of Pt(PF 3) 4 yields of parasitic reactions such as PtCl 2 / Cu. In addition, impurities are difficult to remove, requiring expensive and uncertain additional purification steps. The disclosed method for the robust, high-yield and scalable synthesis of Pt(PF 3) Method 4 can be used at low PF 3 atm (e.g., less than 20 atm) and can be carried out in commonly used commercially available reactors. The disclosed method is a significant advancement in the art to provide a method capable of producing Pt(PF) in high yield. 3) 4 scale-up method, because to date, the potential ideal Pt (PF 3) The precursors have not been used simply because of the lack of scalable synthetic methods. This lack of scalable synthetic methods is due to the fact that the commercially available reactors commonly used for pilot plant synthesis and large-scale manufacturing are not designed for operation at high pressures (e.g., 30 atm or higher) and are not designed for efficient agitation (mixing) of air-sensitive solids, as described above. When the starting material Pt(Hal) 2 (Hal = F, Cl, Br or I) is PtCl 2 and when the metal powder is Cu powder, the disclosed method can be demonstrated for the first time to be used for the reaction of PtCl 2+ PF 3+ Cu synthesis of Pt(PF 3) The reaction of 4 is carried out under reaction conditions (e.g., low pressure from 20 to 300 psig and temperature from 80°C to 130°C) via the sufficiently soluble intermediate PtCl 2(PF 3) 2. Common knowledge is that inorganic compounds such as PtCl 2(PF 3) The solubility of 2 in saturated hydrocarbon solvents is lower than in the aromatic solvent benzene, and therefore calculating the solubility in the hydrocarbon solvent hexadecane is counterintuitive, even for reactions that have such low solubility even in aromatic solvents. Pt(PF 3) 4 Usually according to the prior art, PtCl 2. K 2PtCl 6 and K 2PtCl 6 preparation, and K 2PtCl 6 Need to reduce PF 3 pressure. PtCl 2 and K 2PtCl 6 are both insoluble in the disclosed solvents (e.g., aromatic hydrocarbons, saturated hydrocarbons). As shown in the following examples and comparative examples, for platinum starting compounds, for example, for PtCl 2 (Example 1, surface 1, Comparative Example 1) and for K 2PtCl 6 (Example 7, surface 5) The solvent effect is not similar. Although the addition of the disclosed solvent (e.g., xylene, hexadecane) is effective for the 2 The reaction is beneficial, but in the absence of solvent with the starting compound K 2PtCl Pure reaction of 6: K 2PtCl 6+ Cu(excess) + PF 3(excess) → Pt(PF 3) 4+ 4CuCl + 2KCl than in solvent hexadecane from K 2PtCl The reaction starting from 6 has a higher Pt(PF 3) 4, indicating the solvent benefit for some Pt precursors such as PtCl 2. PtF 2. PtI 2. PtBr 2 etc. are beneficial. Therefore, the solvent is made of Pt(Hal) 2 (Hal = F, Cl, Br or I) synthesis of Pt(PF 3) The 4 Series is novel. picture 1 is an exemplary disclosed method for synthesizing Pt(PF 3) 4 solid-gas PtCl 2+ PF 3+ Cu system block diagram. As shown, first, by pipeline 101 Metal powder such as Cu powder 11 Add to reactor 16. In the disclosed method, an anhydrous solvent is used as a solvent 14. Solvent The solvent used in the present invention may have a water content of from 0 to 50 ppm, preferably from 0 to 10 ppm, more preferably from 0 to 1 ppm. 14 can be dried by contacting with a desiccant selected from 3Å or 4Å molecular sieve or activated alumina. 104 for drying. Drying process 104 can be carried out at a temperature ranging from 10°C to 50°C, preferably at room temperature, for 0.5 to 20 hours. In some embodiments, the drying process 104 can be achieved by keeping the solvent and molecular sieve in the container 15 or by drying process 104 is achieved by passing through a column (not shown) together with a desiccant. After drying, the container The water content of 15 can be determined by Karl Fischer titration or any other suitable analysis. 14 can be a commercially available solvent and can be prepared by applying a vacuum-inert gas cycle or by making the solvent have less than 0.5 ppm of O 2 and moisture inert gas is passed through to degas. Solvent or anhydrous solvent can be 14Store in container 15 or in the drying process 104 immediately after the pipeline 105 leads to the reactor 16. With dry anhydrous solvent 14 containers 15 can be stored or transported to the reactor before the next step 16 other places. Then, under an inert atmosphere (e.g., nitrogen, argon, helium), the solids are added by any suitable means, such as using a solid addition funnel. 102, PtCl 2 12 Loading into the reactor 16. PtCl 2 12 can be anhydrous PtCl 2. In the following, PF 3 13 By pressure difference through the adding pipeline 103 is loaded into the reactor 16, and the reactor 16 can be pre-vacuumed and heated, or at room temperature and pre-vacuumed, or contain PF at a certain pressure and temperature 3. Add PF Before 3, the reactor can be 16. Evacuate to a maximum of 0.1-50 Torr, preferably up to 0.1-2 Torr to remove the inert gas selected from nitrogen, argon, and helium. The absence of non-condensable gases (nitrogen, argon, helium) in 16 will make the product Pt(PF 3) 4 is more efficient. Alternatively, add to the reactor PF in 16 3 can contain 1 atm of nitrogen, argon or helium at room temperature. 3 13 in the reactor 16 is added to the reactor 16 produces PF from 20 psig to 300 psig 3 pressure. PF 3 Can be added gradually or continuously during the process. The value of the 3 pressure depends on the rated pressure of the applied reactor and can be added portionwise or continuously during the process and recycled after the process. reactor 16 can be a device for Pt(PF) with stirring, temperature and pressure control and reaction monitoring devices. 3) Typical vessels for the synthesis and purification of 4. Reactor 16 has cooling and heating means, which are maintained at a temperature ranging from about -120°C to about 200°C, preferably from room temperature to 180°C, more preferably from room temperature to 130°C, and a corresponding pressure ranging from about 10 psig to about 3000 psig, preferably from about 20 psig to about 1000 psig, more preferably from about 20 psig to about 300 psig. Reactor 16 is connected to an empty vessel used as ballast and has a drain port to drain the reaction contents if over pressurized. 16 is connected to nitrogen and vacuum lines (not shown) and PF 3 scrubbers (not shown) and for 107 Collect the product Pt(PF 3) 4 and through pipelines 110 Recycle unreacted PF Trap 3 18 and 20. solvent 14 may include various organic solvents. In some embodiments, the solvent 14 can be a dry alkane solvent selected from decane, dodecane, tridecane, tetradecane, pentadecane or hexadecane. In this case, the Cu powder 11. Anhydrous PtCl 2 12 and dry alkane solvent 14 Loading into the reactor 16 to form a suspension. PtCl 2 solid in solvent The starting amount of 14 is from 1% to 50%, preferably from 5% to 40%, more preferably from 20% to 30%. 2 12 and Cu powder The molar ratio of Pt to Cu is from 1:2 to 1:20, preferably from 1:6 to 1:10. That is, the molar ratio of Pt to Cu is from 1:2 to 1:20, preferably from 1:6 to 1:10. 3 Before 13, the reactor 16. Evacuate to 0.1-50 Torr, preferably 0.2-5 Torr. Alternatively, the solvent 14 can be a dry aromatic solvent selected from xylene, mesitylene, cymene, pentylbenzene, diisopropylbenzene, or diisobutylbenzene. In this case, the Cu powder 11. Anhydrous PtCl 2 12 and dry aromatic solvents 14 Loading into the reactor 16. PtCl The initial amount of solid in the solvent is from 1% to 50%, preferably from 10% to 40%, more preferably from 20% to 30%. The molar ratio of Pt to Cu is from 1:2 to 1:20, preferably from 1:6 to 1:10. That is, the molar ratio of Pt to Cu is from 1:2 to 1:20, preferably from 1:6 to 1:10. 3 Before 13, the reactor 16. Evacuate to 0.1-50 Torr, preferably 0.2-5 Torr. Alternatively, the solvent 14 can be a dry ether solvent selected from dibutyl ether, dihexyl ether, dioctyl ether, diethylene glycol dimethyl ether, triethylene glycol dimethyl ether, tetraethylene glycol dimethyl ether. In this case, the Cu powder 11. Anhydrous PtCl 2 12 and dry ether solvent 14 Loading into the reactor 16. PtCl The initial amount of solid in the solvent is from 1% to 50%, preferably from 10% to 40%, more preferably from 20% to 30%. The molar ratio of Pt to Cu is from 1:2 to 1:20, preferably from 1:6 to 1:10. That is, the molar ratio of Pt to Cu is from 1:2 to 1:20, preferably from 1:6 to 1:10. 3 Before 13, the reactor 16. Evacuate to 0.1-50 Torr, preferably 0.2-5 Torr. In the PF 3 13 Introducing the reactor After 16, the reaction mixture was initially tied to PF 3 PtCl at a pressure of 13 2 12 and Cu powder 11 in solvent 14. The reactor was then heated while stirring the reaction mixture. 16, forming PtCl at a temperature ranging from 20°C to 120°C, preferably at a temperature ranging from 90°C to 120°C 2(PF 3) x (x = 1, 2). After heating for 20-80 minutes under stirring within the above preferred temperature range, the reaction can be stopped and the solvent, reaction by-products, and residual PF can be removed. 3. Separation of PtCl 2(PF 3) 2. Compound PtCl 2(PF 3) x (x = 1, 2) soluble in solvent 14, this can be confirmed with the aid of NMR spectroscopy, e.g. picture 3. The reaction in the reactor 16 in PF 3 continues under pressure, while PF 3 and PtCl 2(PF 3) x (x = 1, 2) dissolved in the solvent and mixed with copper powder 11 reaction. During the reaction process, PF 3 13 is consumed. 3 13 Add to the reactor portion by portion 16 or continuously maintain a constant selected pressure. When all the starting and intermediate platinum compounds are consumed, the reactor The pressure in 16 becomes constant at a given temperature. The reaction time can be in the range of 1 hour to 24 hours, preferably 4 hours to 8 hours. 3. Consumption rate and reactor The pressure changes in 16 are monitored by in situ Raman spectroscopy or any other suitable technique. In some embodiments, the reactor The reaction in 16 was carried out in hexadecane at a PF of 20 to 50 psig. 3, occurs at a temperature of 100°C to 125°C, and is completed within 6 hours. Alternatively, in some embodiments, the reactor The reaction in 16 was carried out in xylene at 20 to 40 psig PF. 3, occurs at a temperature from 100°C to 125°C, and is completed within 5 hours. After the reaction is completed, the reaction mixture is cooled to 20°C to 65°C, preferably 30°C to 45°C. 3. Pt(PF 3) The remaining gas consisting of 4 and solvent is led to a pre-vacuum trap maintained at a temperature ranging from -196°C to -160°C. 17. PF 3 (melting point -151.5°C, boiling point -101.9°C) and Pt(PF 3) 4 (melting point -15 ° C) and solvent in a pre-vacuum trap 17 is condensed. In the pre-vacuum trap 17Pt(PF 3) At the end of condensation, vacuum may be applied periodically to remove residual gases such as nitrogen, argon, and helium to create a vacuum in the range of 0.1 to 50 Torr, preferably 0.2 to 2 Torr, to facilitate the pre-vacuum trap. 17 from the reactor 16 remaining Pt(PF 3) 4. In the distillation of condensation including Pt (PF 3) 4 and PF 3. Before the reaction product, the pre-vacuum trap 17. Pt(PF 3) 4 wells 18 and PF 3 wells 20 is pre-vacuumed to 0.01-10 Torr, preferably 0.1-1 Torr. As an alternative to the procedure described above, after the reaction is completed, the reaction mixture is cooled to 20°C-65°C, preferably 30°C-45°C, and the PF 3. Pt(PF 3) 4 and a portion of the solvent gas is passed through a pipeline maintained at a temperature ranging from -60°C to -80°C. 106 leads to the pre-vacuum trap 17. PF 3 does not condense, and Pt(PF 3) 4 and solvent in a pre-vacuum trap 17 was condensed. 3) 4 and solvent in a pre-vacuum trap After being condensed in 17, the uncondensed PF 3 From the pre-vacuum trap 17 leads to PF maintained within a temperature range of -160°C to -196°C 3 wells 20, then the PF 3. Pt(PF 3) 4 and the next portion of the solvent gas from the reactor 16 Guide to the pre-vacuum trap 17, and the cycle continues until all PF 3 in PF 3 wells 20 is condensed and all Pt(PF 3) 4 In the pre-vacuum trap 17 was condensed. The condensation of the gaseous products is preferably carried out by the steps as described above, wherein a continuous process is disclosed, since even with the use of dry ice-isopropanol (-79°C) on a pre-vacuum trap, the condensation of the gaseous products is not as severe as with the steps described above. 17Effective engineering arrangements and cooling from the reactor 16 The continuous flow of gas will also result in the PF 3 wells 20 bypass 20%-60% Pt(PF) of 108 3) 4, leading to additional steps (not shown) to remove 3 wells 20 Recover all Pt(PF 3) 4. Additional steps may include placing the well 20Warm to above PF 3 boiling point (-102 ° C), usually warmed to -79 ° C (dry ice cooling), and all PF was captured in a first separate trap (not shown) cooled with liquid nitrogen 3. In all PF After all 3 are captured, the trap 20 was warmed to room temperature, and Pt(PF 3) 4 is captured in a second separate trap (not shown). PF captured in the first separate trap 3 can be achieved through pipelines 110 is recycled to PF 3 13 for use in reactors 16. Pre-vacuum trap 17. Pt(PF 3) 4 wells 18 and PF 3 wells 20 and all connecting pipelines are made of metal, wherein the metal material is preferably carbon steel, stainless steel and stainless steel alloy. 17. Pt(PF 3) 4 wells 18 and PF 3 wells 20 and all connecting lines are made of stainless steel. All wells can have passivated or electropolished inner surfaces. Pt(PF 3) 4 and PF 3. After collecting the volatiles, place the pre-vacuum trap 17 warmed to a temperature ranging from -20°C to -90°C, preferably from -60°C to -80°C, and maintained at a temperature ranging from -160°C to -196°C. 3 wells 20 distilled PF 3. PF 3 wells PF in 20 3 can be stored, moved to different locations or used as PF 3 13 was recycled for the next step of synthesis. Pt(PF) contaminated by solvent 3) 4. Reaction by-products such as solid copper chloride in PF 3 After absorption, it is retained in the pre-vacuum trap 17. Pre-vacuum trap Pt(PF) in 17 3) 4 has a purity of 90%-99% and contains 0.1%-5% PF 3 and 0.1-10% of solvent and 0.1%-1% of other impurities, preferably phosphorus oxyfluoride and solid copper chloride. If the mixture is maintained at a temperature ranging from 10°C to 40°C, preferably at room temperature, and the receiver is maintained at a temperature ranging from -50°C to -196°C, and the apparatus and receiver can be pre-vacuumed before distillation, and the pressure during distillation is 0.01 torr to 760 torr, preferably from 0.1 torr to 5 torr, then Pt(PF 3) 4 and the solvent and solid are separated. More specifically, the Pt(PF 3) 4 By using Pt(PF 3) 4 wells 18 and purified by distillation. In one embodiment, in PF 3 After absorption, it will contain Pt(PF 3) 4 pre-vacuum trap 17 Warm to 0°C to 40°C, preferably to room temperature, and place in a pre-vacuum trap 17 wherein Pt(PF) is distilled at a pressure of 0.01-50 Torr, preferably 0.1-2 Torr. 3) 4. At the same time, Pt(PF 3) 4 wells 18 is maintained at a temperature ranging from -15°C to -196°C. In Pt(PF 3) 4 wells Pt(PF 3) 4 has a purity of 70-99.9% w / w, preferably 80-99.9% w / w, more preferably 90-99.9% w / w, even more preferably 95-99.9% w / w, even more preferably 99.0-99.99% w / w after purification. Preferably, the collected Pt(PF 3) 4 has a purity of 99.50-99.99% w / w and contains 0%-0.5% PF 3. 0.01%-0.5% of other impurities (such as phosphorus oxyfluoride), thermal decomposition products (such as Pt 4(PF 3) 8) and 0%-0.5% residual solvent. 1 H. 19 F. 31 P. 195 Pt NMR, FTIR and Raman spectroscopy were used to determine the Pt(PF 3) 4 in purity. Purified Pt(PF 3) 4 can have a PF from about 0 wt.% to about 0.1 wt.% 3, preferably from about 0 wt.% to about 0.05 wt.% PF 3 impurities. Purified Pt(PF 3) 4 may have between about 0 wt.% and about 1 wt.%, preferably between about 0 wt.% and about 0.05 wt.% including PF 3. POF 3. (HO)POF 2. (HO) 2POF phosphorus fluoride and oxyfluoride. Purified Pt(PF 3) 4 may have between 0 wt.% and about 0.1 wt.% other than Pt (PF 3) 4. Preferably, from about 0 wt.% to about 0.05 wt.% is not Pt(PF 3) 4 platinum compounds. After purification, Pt(PF 3) 4 Pt(Hal) 2. Pt 4(PF 3) 8. Pt(Hal) 2(PF 3) x The total concentration of (Hal = F, Cl, Br or I, x = 1, 2) can be from about 0 wt.% to about 0.1 wt.%, preferably from about 0 wt.% to about 0.05 wt.%. In addition, the purified Pt(PF 3) 4 may have between 0.1 ppmw and 1000 ppmw of solvent used for the synthesis, preferably from about 0 ppmw to 200 ppmw of solvent, more preferably from 0 ppmw to 50 ppmw of solvent, and even more preferably from 0 ppmw to 20 ppmw of solvent. In addition, the purified Pt(PF 3) 4 can have from about 0 ppmw to about 100 ppmw of hydrogen fluoride, from 0 ppmw to about 50 ppmw of hydrogen chloride. In addition, the purified Pt(PF 3) 4 may have trace metals such as iron, nickel, manganese, cobalt, copper, etc. between about 0 ppb and 10 ppm. 3 Recycled for Pt(PF 3) 4 synthesis. In some embodiments, to determine the Pt(PF 3) 4. The amount of organic compounds can be measured using an internal standard such as Me 4Si. In some embodiments, sample preparation may involve the use of an appropriate adsorbent such as C 8 derived silica gel) absorbs organic solvents. In some embodiments, Pt(PF 3) 4 wells 18 may include two subsequent traps, for example, a trap for distillation 18a and well 18b (not shown) to obtain Pt(PF) of desired purity 3) 4. After purification, it is packaged in metal ampoules 19 Before transportation, placement or storage, Pt(PF 3) 4 can be stored in Pt(PF 3) 4 wells 18. Alternatively, in the packaging After 109, Pt(PF 3) 4 can be stored in metal ampoules 19. Metal ampoule 19 can be a metal container / vessel made of metal (such as stainless steel, carbon steel and stainless steel 316 alloy). Metal ampoule The inner surface of 19 can be made of PF 3. Passivation or electropolishing. In the case of Pt(PF 3) 4Introduction of metal Pt(PF 3) 4 wells 18 metal ampoules 19, the Pt(PF) metal can be removed by heating at about 100°C to 170°C under vacuum. 3) 4 wells 18. Metal ampoule 19. Alternatively, in the case of Pt(PF 3) 4Introduction of metal Pt(PF 3) 4 wells 18 metal ampoules Before 19, you can use PF 3. Passivation well vessel removes Pt(PF 3) 4 wells 18. Metal ampoule 19. Surface moisture. Purified Pt(PF 3) 4 can be stored in a metal Pt (PF) in a temperature range of -80°C to 60°C, preferably from 10°C to 40°C, more preferably from 20°C to 25°C. 3) 4 wells 18. Metal ampoule 19. The disclosed method comprises the following steps: 3) 4 Store in metal containers, such as stainless steel, carbon steel and stainless steel 316 alloy containers. The inner surface of the metal container can be PF 3 passivation or electropolishing. Here, the stainless steel container can be a stainless steel single-ended micro sample cylinder or an electropolished stainless steel micro tank. In an exemplary embodiment, the purified Pt (PF 3) 4 was stored in a stainless steel single-ended micro-sample cylinder at room temperature for 2 months while Pt(PF 3) The purity of 4 was unchanged. Alternatively, the purified Pt(PF 3) 4 were stored in electropolished stainless steel micro-cans at room temperature for 2 months while Pt(PF 3) The purity of 4 remains unchanged. The disclosed method can be carried out by using a soluble intermediate Pt(Hal) 2(PF 3) x (x = 1, 2; Hal = F, Cl, Br or I) (e.g. picture The so-called solid-gas, Pt(Hal) shown in 2a 2-M-PF 3) The steps of the synthesis process in solution are shown. Here, HAL is F, Cl, Br or I, preferably Hal is Cl; M is a metal (such as Cu), then Pt(Hal) 2-M-PF 3 Synthesis process becomes PtCl 2-Cu-PF 3 Synthesis process. The disclosed method produces Pt(PF) with high yield (i.e., 70% to 99.9%) and high purity (i.e., greater than 99%, preferably greater than 99.99%). 3) 4, and allows the storage and delivery of high-purity Pt(PF 3) 4 without reducing the purity. Using hydrocarbon solvents for the disclosed solid-gas PtCl 2-Cu-PF 3. The reaction process is advantageous in which the solvent is capable of dissolving the solid platinum compound PtCl from the insoluble starting material under appropriate reaction conditions. 2 and PF 3 gas-formed reaction intermediates (e.g., platinum complex PtCl 2(PF 3) 2) and not with Pt(PF 3) 4 reaction. The use of this solvent allows the 3. Obtain Pt(PF) in a shorter time and with higher yield under high pressure 3) 4. Due to the Pt(PF 3) PF in the synthesis method of 4 3 lower pressure, eliminating the need to cool the reactor to condense PF 3, and reactors with lower pressure ratings can be used. Therefore, commonly available equipment and reactors can be used for the disclosed Pt(PF 3) 4. This leads to the synthesis of Pt(PF 3) 4 The synthesis method can be expanded to a large industrial scale with limited equipment complexity due to its lower pressure requirement. Here, the reaction conditions include reaction temperature, reaction pressure, etc. Using the disclosed synthesis method, by 2-Cu-PF The addition of the disclosed solvent to the reaction system solves the low, moderate and irreproducible yields in solid-gas reactions and the problems of the synthesis of Pt(PF 3) 4 PF required 3. The high pressure problem. The addition of solvent allows the Synthesis of Pt(PF) in a shorter time and with reproducible high yield under 3 pressures 3) 4 ( surface 1, Examples #1 to #4). The reason for the improvement in the synthesis method is that PtCl 2 and PF 3 In situ obtained PtCl 2(PF 3) 2. It is common knowledge that solution-solid reactions are much more efficient than reactions between two different solids and gases. The addition of solvent makes solid-gas PtCl 2-Cu-PF 3 reaction system into a much more efficient solution-solid reaction. Although the use of solvents in synthesis is common practice, due to the reaction conditions used, PF The high reactivity of 3, along with the Pt-rich coordination and catalytic chemistry in organic solvents, is not an obvious solution for the given reaction system and may even be argued against. In solid-gas Pt(Hal) 2-M-PF 3. Addition of solvent to the synthesis system solves the problem of low, moderate and irreproducible yields in solid-gas reactions (see Comparative Example 1 below) and for the synthesis of Pt(PF 3) 4 PF required 3. High pressure (50 - 150 Atm) problem. The addition of solvent allows the Synthesis of Pt(PF) in a shorter time and with reproducible high yield under 3 pressures 3) 4, see Examples 2 to 4 below. The reason for the improved yield is that under certain reaction conditions, PtCl 2 and PF 3 In situ obtained reaction intermediate PtCl 2(PF 3) Solubility of 2 ( picture 3). Again, solution-solid reactions are known to be much more efficient than reactions between two different solids and a gas. In Examples 2 to 4 below, in the case of PtCl 2-Cu-PF 3 Addition of solvent to the synthesis system allows for PF values between 10 and 50 psig Pt(PF) was synthesized in reproducible high yields within 5 to 6 hours under 3 pressure. 3) 4 (see also Example 1), because solid-gas PtCl 2-Cu-PF 3 synthesis system into a solution-solid reaction. Therefore, commonly available equipment and reactors can be used for the disclosed Pt (PF 3) 4. Synthesis method of 4. The appropriate solvent should be tolerant to the starting compounds, intermediates and product Pt(PF 3) 4 is "inert" and does not react with the starting compounds, intermediates, and product Pt(PF) under the reaction conditions. 3) 4 reaction. In other words, the appropriate solvent should not be reacted with the starting compound, intermediate and product Pt(PF) under the reaction conditions. 3) 4 catalytic conversion, and the solvent should not convert the starting compound and product into other compounds. A suitable solvent should only dissolve at least one intermediate in the reaction to obtain a solution-solid reaction, which is much more efficient, reproducible and therefore scalable than a reaction between two different solids and a gas. A suitable solvent should be able to dissolve the Pt(Hal) 2 and PF 3. At least one platinum-containing reaction intermediate obtained in situ, such as Pt(Hal) 2(PF 3) x , where Hal = F, Cl, Br or I; x = 1, 2. Platinum precursors can form soluble reaction intermediates in the solvent under certain reaction conditions. Otherwise, the addition of solvent will result in a decrease in the concentration of Pt(PF) compared to the reaction without solvent. 3) 4, see where Pt(PF 3) 4 yield of 60% of Comparative Example 1 (b)), and the Pt (PF 3) The yield of 4 is 26% of Example 7 (#9). The disclosed platinum precursor Pt(Hal) 2 (Hal = F, Cl, Br or I) form soluble intermediates, and therefore they are suitable for the disclosed synthetic methods. The suitable solvent used herein can be selected from ether, aromatic hydrocarbon or alkane solvent. The boiling point (BP) of the solvent is preferably greater than 150°C, preferably greater than 200°C. This is for the solvent and the product Pt (PF 3) 4 is necessary because Pt(PF 3) The calculated boiling point of 4 is about 77°C, calculated from "Vapor Pressure Measurements of Volatile Transition-Metal Complexes" by RD Sanner, JH Satcher, Jr., Report (1989), UCRL-53937, according to the equation logP = 10.34-2610 / T (P is in Torr, T is in Kelvin). For example, hexadecane (BP: 285°C, melting point (MP): 18°C and vapor pressure (VP): 0.07 Torr at 20°C), p-cymene (BP: 177°C, MP: -68°C and VP: 1 Torr at 20°C), and dihexyl ether (BP: 223°C, MP: -43°C and VP: 0.05 Torr at 20°C), triethylene glycol dimethyl ether (BP: 216°C, MP: -45°C and VP: 0.025 Torr at 20°C), tetraethylene glycol dimethyl ether (BP: 275°C, MP: -30°C and VP: 0.001 Torr at 20°C) can be suitable for use as the disclosed Pt(Hal) 2-M-PF 3. Solvents in the synthesis system. In one embodiment, from PtCl 2 and PF 3 Isolation of the intermediate PtCl in the reaction in hexadecane 2(PF 3) 2. Confirm the identity by analysis. 2(PF 3) 2 Further with copper and PF 3 in surface 1 under the conditions disclosed in #5 to produce Pt(PF 3) 4. Pt(PF 3) The synthesis of 4 must use anhydrous solvents because PF 3. PtCl 2. PtCl 2(PF 3) x (x = 1, 2) and Pt(PF 3) 4. Reacts with moisture. The reaction with moisture produces by-products such as HCl, HF, and / or phosphorus oxyfluoride, fluorophosphoric acid, which contaminate the product Pt (PF 3) 4. For example, when Pt(PF 3) 4 When placed in any container made of glass, HF can form SiF 4. To prevent the formation of contaminants, commercially available solvents can be dried by contact with a drying agent. picture 2a is disclosed for using Pt(Hal) 2 (Hal = F, Cl, Br or I) to start the synthesis of Pt(PF 3) 4Pt(Hal) 2-M-PF 3. Flowchart of the synthesis method. The starting materials include Pt(Hal) 2 (Hal = F, Cl, Br or I) and metal powder (M) and PF 3. In the reaction temperature range of 20°C-180°C, Pt(Hal) 2 (Hal = F, Cl, Br or I) and metal powders can be insoluble. For example, PtCl 2 is insoluble at reaction temperatures ranging from 20°C to 180°C. First, in step 202, by Pt(Hal) 2 (Hal = F, Cl, Br or I) and metal powder are dispersed in an anhydrous solvent to form the starting material Pt(Hal) in an anhydrous solvent 2 (Hal = F, Cl, Br or I) and metal powder suspension. Then, excess PF 3Gas introduction Pt(Hal) 2 (Hal = F, Cl, Br or I) and metal powder suspension. Here, preferably, Hal = Cl, then Pt(Hal) 2-series PtCl 2. Preferably, the metal powder is Cu powder. Pt(Hal) 2 (Hal = F, Cl, Br or I) is anhydrous and is suspended in an anhydrous solvent. The solvent is dried by a drying agent to form an anhydrous Pt(Hal) 2 and the metal powder mixed with an anhydrous solvent. The solvent or anhydrous solvent can be a hydrocarbon solvent, such as a solvent having the general formula (C n H 2n+1 ) 2O and H 3C(O(CH 2) 2) n OCH 3 (n ≥ 1) oxygenated hydrocarbon solvent, having the general formula (C n H 2n+1 ) x C 6H 6-x (x ≥ 1, n ≥ 1) aromatic solvent or a solvent having the general formula C n H 2n+2(n ≥ 1) alkane solvent. Anhydrous solvents suitable for use in the disclosed method can be dry alkane solvents selected from decane, dodecane, tridecane, tetradecane, pentadecane, and hexadecane; dry aromatic hydrocarbon solvents selected from xylene, mesitylene, cymene, pentylbenzene, diisopropylbenzene, and diisobutylbenzene; dry ether solvents selected from dibutyl ether, dihexyl ether, dioctyl ether, diethylene glycol dimethyl ether, triethylene glycol dimethyl ether, and tetraethylene glycol dimethyl ether; or aromatic hydrocarbon solvents selected from xylene, mesitylene, cymene, pentylbenzene, diisopropylbenzene, and diisobutylbenzene; or combinations thereof. Ether solvents are preferably dibutyl ether, dihexyl ether, dioctyl ether, triethylene glycol dimethyl ether, and tetraethylene glycol dimethyl ether. Aromatic hydrocarbon solvents are preferably xylene, mesitylene, cymene, pentylbenzene, diisopropylbenzene, and diisobutylbenzene. The alkane solvent is preferably dodecane, tridecane, tetradecane, pentadecane and hexadecane and a mixture of alkanes known as mineral oil. The anhydrous solvent used in the disclosed method can be xylene or hexadecane. In some embodiments, the solvent or anhydrous solvent can be xylene or hexadecane. The drying agent can be a 3 Å or 4 Å molecular sieve. 204, Pt(Hal) 2 (Hal = F, Cl, Br or I), metal powder and excess PF 3. A soluble reaction intermediate Pt(Hal) can be formed in anhydrous solvents 2(PF 3) x (x = 1, 2; Hal = F, Cl, Br or I). The solvent or anhydrous solvent used in this article must be able to dissolve Pt(Hal) 2(PF 3) x (x = 1, 2; Hal = F, Cl, Br or I), a soluble reaction intermediate. Here, the excess PF 3 added to Pt(Hal) 2 (Hal = F, Cl, Br or I) and metal powder in a suspension. Therefore, the soluble reaction intermediate Pt(Hal) 2(PF 3) x (x = 1, 2; Hal = F, Cl, Br or I) can be made of Pt(Hal) 2 (Hal = F, Cl, Br or I) and excess PF 3 is formed at a temperature between 80°C and 130°C and a low pressure between 20 psig and 300 psig. Since the solvent is selected to be able to dissolve the intermediate Pt(Hal) 2(PF 3) x (x = 1, 2; Hal = F, Cl, Br or I), so Pt(Hal) 2 (Hal = F, Cl, Br or I) with excess PF 3. Reaction can produce reaction intermediate Pt(Hal) 2(PF 3) x (x = 1, 2; Hal = F, Cl, Br, or I) in an anhydrous solvent. 206, reaction intermediate Pt(Hal) 2(PF 3) x (x = 1, 2; Hal = F, Cl, Br or I) can be mixed with metal powder and PF 3 Gas reaction (for example, when Hal = Cl, the metal powder is Cu powder, PtCl 2(PF 3) 2+ 2Cu + 3PF 3 = 2CuCl + Pt(PF 3) 4) to form Pt(PF 3) 4. In this step, use excess PF 3. Then, in step 208, the generated Pt(PF 3) 4 with unreacted starting materials, solvents, and reaction by-products such as copper halides (e.g., CuCl, CuCl 2) and its relationship with PF The separation and purification steps can be carried out in a pre-vacuum trap and / or a metal trap to remove residual PF 3 and solvents and reaction by-products, such as picture 1. Residual PF 3 can be recycled to be used as starting material. The metal trap can be made of metals such as stainless steel, carbon steel and stainless steel 316 alloy. Then in step 210 The purified product Pt(PF 3) 4 Store in a metal ampoule or vessel or container. The storage ampoule or vessel or container can be made of metal, such as stainless steel, carbon steel, and stainless steel 316 alloy. Alternatively, the storage ampoule or vessel or container can be made of plastic. The inner surface of the ampoule or vessel or container can be made of PF 3. Passivation or electropolishing. In the disclosed method, Pt(PF 3) The synthesis of 4 must use anhydrous solvents because PF 3. PtCl 2. PtCl 2(PF 3) x (x = 1, 2) and Pt(PF 3) 4 reacts with moisture. To prevent the formation of contaminants, the commercially available solvent can be dried by contacting it with a desiccant selected from 3 Å or 4 Å molecular sieves or activated alumina. The solvent drying process can be achieved by contacting the solvent and the desiccant, which can be achieved in a static process or in a flow process. Prior to the drying step, the commercially available solvent can be degassed by passing an inert gas through it or by applying a vacuum-inert gas cycle, wherein the vacuum is in the range of 0.1 torr to 100 torr, preferably 0.5-10 torr, and the inert gas is selected from N containing less than 1 ppm of oxygen and moisture. 2. Ar or He. Alternatively, commercially available solvents were dried with a desiccant without degassing. The disclosed synthesis method is beneficial to the product Pt(PF 3) The high yield of 4 and the reaction conditions that minimize the impact of side reactions provide Pt(PF 3) The disclosed synthetic methods can be performed in standard high-pressure reactors, such as the 1900 to 5000 psig rated reactors from Parr Instrument Company series 4520, 4530, 4540, 4540; in pressure-rated glass reactors, such as the 5100 glass reactor from Parr Instrument Company rated up to 150 psig; or in laboratory and pilot pressure reactors from Büchiglas equipped with standard stirrers and heaters. In some embodiments, the disclosed methods for Pt(PF 3) The synthesis, purification and storage of 4 may include the following steps: a) drying the solvent; b) reacting a compound having the general formula Pt(Hal) in a flow reactor; 2 (Hal = Cl, Br, I) platinum compounds (such as PtCl 2) and metal powder with a certain particle size (such as copper powder) dispersed in a dry or anhydrous solvent to form Pt(Hal) 2 (Hal = Cl, Br, I) and a mixture or suspension of metallic copper powder; c) excess PF 3 is added to the mixture or suspension; d) at the desired temperature and desired PF to result in the following reaction and product 3 pressure (ie, low PF 3 pressure) stirring the reaction mixture formed in step c) : a. PtCl 2(PF 3) x (x = 1, 2); b. Formation of PtCl 2(PF 3) x A solution in a dry solvent; and c. PtCl 2(PF 3) x and PF 3 reacts with metallic copper powder to form the product Pt(PF 3) 4; e) purifying the product Pt(PF) by distilling the volatiles from the reaction mixture into a separate trap 3) 4, which allows: i. separation of one or more unreacted starting materials, by-products, solvents; and ii. separation of the product Pt(PF 3) 4 and unreacted PF 3. f) Purification of crude Pt(PF) by distillation 3) 4; g) unreacted PF 3 is recycled to step c); and h) the purified product Pt(PF 3) 4 Stored in a metal ampoule or container made of metal such as stainless steel, carbon steel and stainless steel 316 alloy, and the inner surface of the metal ampoule or container is 3. Passivation or electropolishing. Alternatively, the disclosed method for using a platinum compound Pt(Hal) 2 (where Hal = F, Cl, Br or I) to synthesize Pt(PF 3) The method of claim 4 comprises the following steps: 2 (where Hal = F, Cl, Br or I) dispersed in an anhydrous solvent to form Pt(Hal) 2 suspension; excess PF 3Introduction of Pt(Hal) 2 in suspension; by PF 3 and Pt(Hal) 2 reaction to form a platinum compound Pt(Hal) 2(PF 3) x A solution in an anhydrous solvent; a metal powder having a certain particle size and an excess of PF 3 added to Pt(Hal) 2(PF 3) x solution; and under reaction conditions by Pt(Hal) 2(PF 3) x PF 3 reacts with the metal powder to form Pt(PF 3) 4. In this case, Pt(Hal) 2(PF 3) x Excessive PF 3 and Pt(Hal) 2 in anhydrous solvent suspension synthesis of the reaction intermediates. Again, the use of solvents for the synthesis of Pt (PF 3) 4 appears to be novel. As far as we know, Pt(PF 3) 4 has never been synthesized from any platinum compound, including the reaction intermediate Pt(Hal) in solvent 2(PF 3) x (Hal = F, Cl, Br or I; x = 1, 2). Alternatively, the disclosed method for using a platinum compound Pt(Hal) 2 (where Hal = F, Cl, Br or I) to synthesize Pt(PF 3) The method of claim 4 comprises the following steps: providing a metal powder having a certain particle size; providing a PF 3 gases; in the metal powder, PF 3 and platinum compounds Pt(Hal) 2 (where Hal = F, Cl, Br or I) in anhydrous solvent to synthesize Pt(PF 3) 4. The anhydrous solvent is capable of dissolving at least one platinum-containing reaction intermediate Pt(Hal) 2(PF 3) x (Hal = F, Cl, Br or I; x = 1, 2), which is composed of a platinum precursor Pt(Hal) 2 and PF 3 is formed under reaction conditions such as low pressure from 20 psig to 300 psig and temperature ranging from 80°C to 130°C; and Pt(PF) is purified and stored in devices and ampoules made of metal or plastic under air and moisture free conditions. 3) 4. Alternatively, the disclosed method for using a platinum compound Pt(Hal) 2 (where Hal = F, Cl, Br or I) to synthesize Pt(PF 3) The method of claim 4 comprises the following steps: a) drying the solvent with a desiccant to form an anhydrous solvent; b) mixing a metal powder having a certain particle size and a general formula of Pt(Hal) 2 (where Hal = F, Cl, Br or I) platinum compounds and excess PF 3 is added to anhydrous solvent to form Pt(Hal) 2(PF 3) x (where x = 1, 2), where the anhydrous solvent can dissolve Pt(Hal) 2(PF 3) x ; c) by metal powder, PF 3 and Pt(Hal) 2(PF 3) x Synthesis of Pt(PF 3) 4; and d) purification of the synthesized Pt(PF 3) 4 and the purified Pt(PF 3) 4 Store in air- and moisture-free containers and ampoules made of metal or plastic, such as stainless steel or plastic. Here, the plastic may be selected from polyethylene, polypropylene, styrene, Teflon, polytetrafluoroethylene (PTFE), and perfluoroalkoxyalkane (PFA). As described above, the reaction intermediate Pt(Hal) 2(PF 3) x (Hal = F, Cl, Br or I; x = 1, 2) are soluble in hydrocarbon solvents and can be isolated and purified. Pt(PF 3) The synthesis of 4 can be done with the platinum compound Pt(Hal) 2(PF 3) x (Hal = F, Cl, Br or I, x = 1, 2). picture 2b series uses Pt(Hal) 2(PF 3) x (x = 1, 2; Hal = F, Cl, Br or I) to start the synthesis of Pt(PF 3) 4 is a flow chart of an exemplary method. As shown, in step 302, Pt(Hal) 2(PF 3) x (Hal = F, Cl, Br or I; x = 1, 2) solution by adding Pt(Hal) 2(PF 3) x (Hal = F, Cl, Br or I; x = 1, 2) is dissolved in an anhydrous solvent. Preferably, Hal is Cl, Pt(Hal) 2(PF 3) x PtCl 2(PF) x Then in step 304, introducing metal powder with a certain particle size into Pt(Hal) 2(PF 3) x (Hal = F, Cl, Br or I; x = 1, 2) solution to form a suspension. Preferably, the metal powder is Cu powder with a certain particle size. Then, in step 306 will be excessive PF 3. Gas is introduced into the suspension. Then, in step 308, under low pressure by making Pt (Hal) 2(PF 3) x (x = 1, 2; Hal = F, Cl, Br or I) with metal powder and PF 3 reaction to form Pt(PF 3) 4. In this step, use excess PF 3. Then, in step 310, the generated Pt(PF 3) 4 with unreacted starting materials, solvents, and reaction by-products such as copper halides (e.g., CuCl, CuCl 2) and its relationship with PF The separation and purification steps can be carried out in a pre-vacuum trap and / or a metal trap to remove residual PF 3 and solvents and reaction by-products, such as picture 1. Residual PF 3 can be recycled to be used as starting material. The metal trap can be made of metals such as stainless steel, carbon steel and stainless steel 316 alloy. Then in step 312 The purified product Pt(PF 3) 4 Store in a metal ampoule or vessel or container. The storage ampoule or vessel or container can be made of metal, such as stainless steel, carbon steel, and stainless steel 316 alloy. Alternatively, the storage ampoule or vessel or container can be made of plastic. The inner surface of the ampoule or vessel or container can be made of PF 3. Passivation or electropolishing. The disclosed method for using a platinum compound Pt(Hal) 2(PF 3) x (where Hal = F, Cl, Br or I; x = 1, 2) to synthesize Pt(PF 3) The method of 4 comprises the following steps: Pt(Hal) 2(PF 3) x (Hal = F, Cl, Br or I; x = 1, 2) dissolved in anhydrous solvent to form Pt(Hal) 2(PF 3) x Solution; Metal powder with a certain particle size and excess PF 3 added to Pt(Hal) 2(PF 3) xsolution; and under reaction conditions of low pressure ranging from 20 psig to 300 psig and temperature ranging from 80 ° C to 130 ° C, by Pt (Hal) 2(PF 3) x PF 3 and the metal powder to form Pt(PF 3) 4. Alternatively, the disclosed method for using a platinum compound Pt(Hal) 2(PF 3) x (where Hal = F, Cl, Br or I; x = 1, 2) to synthesize Pt(PF 3) The method of claim 4 comprises the following steps: a) drying the solvent with a desiccant to form an anhydrous solvent; b) adding a platinum compound Pt(Hal) 2(PF 3) x (where Hal = F, Cl, Br or I; x = 1, 2), metal powder with a certain particle size and excess PF 3 was added to anhydrous solvent to synthesize Pt(PF 3) 4. The anhydrous solvent can dissolve Pt(Hal) 2(PF 3) x ; and c) purification of the synthesized Pt(PF 3) 4 and the purified Pt(PF 3) 4 Store in air- and moisture-free containers and ampoules made of metal or plastic such as stainless steel. Here, the plastic may be selected from polyethylene, polypropylene, styrene, Teflon, polytetrafluoroethylene (PTFE), and perfluoroalkoxyalkane (PFA). The metal may be selected from carbon steel, stainless steel, or 316 stainless steel alloy. The metal powder may be Cu, Zn, or Al powder, etc. The present disclosure also includes the product Pt(PF 3) 4 purity and the product Pt(PF 3) 4 storage container. Product Pt (PF 3) 4 can be stored in stainless steel and electropolished stainless steel containers at room temperature without purity change. 3) The method of claim 4 further comprises purifying the synthesized Pt(PF 3) Step 4: Distillation of the synthesized Pt(PF) in a metal trap 3) 4 to remove the solvent and by-products to form by-product-removed Pt(PF 3) 4. Pt(PF) removed by distillation of by-products in metal containers 3) 4. To remove solvent and residual PF 3. Formation of purified Pt(PF 3) 4; and if necessary, the remaining PF 3 Recycled for the synthesis of Pt(PF 3) 4. The disclosed method for synthesizing Pt(PF 3) The method of claim 4 further comprises storing the purified Pt(PF 3) Step 4: Purified Pt(PF 3) 4 Store in metal (e.g., stainless steel) containers or metal (e.g., stainless steel) containers with passivated or electropolished inner surfaces. Here, the purified Pt(PF) stored in a metal container or a metal container with a passivated or electropolished inner surface is 3) The purity of 4 may not change and remain constant. The vessels are made of carbon steel, stainless steel and stainless steel 316 alloy. The metal vessels may have an electropolished inner surface. Alternatively, Pt(PF 3) 4. Can be stored in plastic containers. The plastic material can be polyethylene, polypropylene, styrene, Teflon, polytetrafluoroethylene (PTFE), perfluoroalkoxyalkane (PFA). The metal powder used in the disclosed method is composed of a metal having an electrode potential lower than that of platinum and not reacting with PF under the reaction conditions. 3 interacts with and does not interact with PF 3 forms a complex and has a metal composition that allows it to remain in powder form during the reaction process. The metal powder is preferably copper, zinc, aluminum powder, etc. In this paper, it is possible to use powders that do not react with PF under the reaction conditions. 3 interacts with and does not interact with PF 3 Any metal and its halide that forms a complex and has an electrode potential lower than that of platinum (+1.2). For example, Cu (+0.34), Pb (-0.13), Sn (-0.14), Cd (-0.40), Zn (-0.76) and their halides do not react with PF under the reaction conditions. 3 interacts with and does not interact with PF 3 to form a complex, which can be used as a metal powder. Examples The following non-limiting examples are provided to further illustrate embodiments of the present invention. However, these examples are not intended to be all-inclusive and are not intended to limit the scope of the invention described herein. Experimental procedures The reaction mixture, starting materials, solvents and products can be analyzed by any suitable means, such as by gas chromatography, NMR, Raman, FTIR spectroscopy, using a portion of the stream or an aliquot. All measurements are performed on samples in closed containers, suitable tubes, or ampoules without any contact with an atmosphere containing oxygen and moisture. Liquid nitrogen, with less than 0.1 ppm of O 2 and water of high purity nitrogen. Reagent: Potassium hexachloroplatinate (IV) (K 2PtCl 6, Pt determined to be 40.1 ± 0.7%, CAS: 16921-30-5) from Colonial Metals, Inc.; platinum(II) chloride (PtCl 2, Pt determined to be 73.3 ± 1.0%, CAS: 10025-65-7) from Colonial Metals, Inc. Three types of copper powder, one (99.999%) 100 mesh (100 mesh = 149 µm) from Strem Chemicals Inc.; another < 425 μm, 99.5% from Sigma-Aldrich; and another < 45 μm, 99.99% from Sigma-Aldrich. Phosphorus(III) fluoride (PF 3, CAS: 7783-55-3) were obtained from Advance Research Chemicals, Inc. 3 Å, beaded, 4-8 mesh molecular sieves (Sigma-Aldrich) were regenerated in a dry nitrogen stream at 300°C-350°C or under vacuum at 300°C-350°C and after regeneration were heated in a humidified atmosphere with 0.5 ppm of O The operation was carried out under a nitrogen atmosphere with 2% and no moisture. Solvents xylene and hexadecane were from Sigma-Aldrich, degassed and dried over 3 Å molecular sieves. 2 and water in a nitrogen atmosphere, the reactor was loaded with platinum compound and copper powder. Examples 1. Synthesis of Pt(PF) in a high-pressure reactor using hexadecane solvent 3) 4. Refer to the following surface 1. In a glove box, a certain amount of PtCl 2. Cu and hexadecane were loaded into a reactor from Parr Instrument Company (series 4540, 600 mL, rated at 5000 psig). The reactor was transferred and connected to a vacuum line, evacuated to less than 0.3 Torr and the required amount of PF was added at less than -79°C (# 1-3) or at room temperature (# 6). 3 was introduced into the reactor. The reactor was then warmed to room temperature, stirring was started, and the temperature in the reactor was then raised to 105°C and the reaction mixture was heated in a PF 3 pressure. In reaction #6, PF 3 was added to the reactor portionwise to maintain the pressure in the range of 100 - 200 psig. A pressure drop was observed in all reactions during the first 6 hours at 105°C, and then the pressure stabilized, indicating that the reactions could take about 6 hours. The pressure in the reactor was monitored over a few more hours, and then the reactor contents were cooled to 35°C - 45°C, and a portion of the gas (about 25% - 35%) was directed into a pre-vacuum trap (0.44 L, material stainless steel) cooled with a dry ice-isopropanol mixture. In reaction #6, all pressure was released in the trap. The reactor was closed, the trap was held for about 10 min, and then the non-condensable gases were directed into a second trap (6 L, material aluminum) cooled with liquid nitrogen. If cooled to below 0°C with the passing gas, the transfer lines and valves were warmed. PF in the 6 L Al trap After 3 partial condensation, apply vacuum to the 6 L Al trap to make the pressure in the trap below 1 Torr. Repeat the operation until all PF 3 and Pt(PF 3) 4 was stripped from the reactor and collected in two different traps. 3) The well of 4 was reconnected to a separate pre-vacuum vessel (0.4 L, electro-polished stainless steel). 3) The precursor well of 4 was warmed to room temperature while the receiving vessel was cooled with liquid nitrogen and all the Pt(PF) was distilled in the receiving vessel under static vacuum. 3) 4. After distillation, the receiving vessel was warmed to room temperature and the residual PF 3 released by the scrubber. Pt(PF 3) The yield of 4 is below surface 1 in. [ surface 1] *Reaction 6 is indicative. SS Steel Reactor = High Pressure Reactor (Series 4540, 600 mL) from Parr Instrument Company. Glass Reactor = 150 mL HW Pressure Glassware, from Chemglass Life Sciences, Part No. CG-1880-31. Glassware equipped with thermocouple and pressure gauge. according to 1 H. 19 F NMR, in all experiments Pt(PF 3) The purity of 4 is greater than 99%. For example, in reaction #1, the pure product 19 F NMR (σCFCl 3, ppm): -11.5 (m, J(PF) = 1302 Hz, 99.63%, Pt(PF 3) 4), -34.4 (d, J(PF) = 1402 Hz, 0.05%, PF 3), -81.58 (0.19%, fluorophosphoric acid, unspecified), -92.4 (d, J(PF) = 2035 Hz, 0.12%, POF 3). Pure product 1 H NMR (σSiMe 4, ppm): 0.90 and 1.32 (hexadecane), 13.1 (s, fluorophosphoric acid). 1 H NMR confirmed hexadecane. 0.18 g of the purified product from reaction #1 was mixed with 0.77 g of a 0.03% (0.23 mg, 0.0026 mmol) SiMe 4) C 6D 6. Mix the solution 1 H NMR (σSiMe 4, ppm): 0.00 (s, 97.7 mol.%, SiMe 4), 1.32 (2.3 mol.%, hexadecane), 7.16 (s, fluorophosphoric acid, due to C 6D 6 The relative intensities were not measured because the water was not removed). If, in order to recalculate the mol% to wt.%, the solution is calculated to contain 0.23 mg TMS, then Pt(PF 3) The total amount of hexadecane in the sample 4 was 0.014 mg, corresponding to the Pt(PF 3) 79 ppm in 4. Additional well-to-well distillation yielded Pt(PF) with a purity of 99.79%. 3) 4. Pure samples measured in glass ampoules 19 F NMR (σCFCl 3, ppm): -11.5 (m, J(PF) = 1302 Hz, 99.79%, Pt(PF 3) 4), -88.20 (d, J(PF) = 975 Hz, 0.19%, (HO)POF 2), -92.4 (d, J(PF) = 2035 Hz, 0.01%, POF 3) -166.1 (s, 0.02%, SiF 4). Pure sample 1 H NMR (σSiMe 4, ppm): 0.90 and 1.32 (hexadecane, relative intensity 28%), 12.94 (s, (HO)POF 2, relative intensity 72%). The resonance of hexadecane is lower than that of 0.07 g of sample in the presence of 0.03% SiMe 0.78 g of C 6D 6. Therefore, the total amount of hexadecane is less than 80 ppm. FTIR. [Liquid Pt(PF 3) 4 on Golden Gate™ probe, resolution 4 cm -1 ]: 882, 827, 496 cm -1 . Examples 2. Separation of PtCl 2(PF 3) 2 and hexadecane solvent to synthesize Pt(PF 3) 4. a) Synthesis of PtCl in hexadecane 2(PF 3) x (x = 1, 2). PtCl 2 (1.9 g, 7.1 mmol) and hexadecane (15.8 g, 20.4 mL) were loaded into a 150 mL pressure glass ampoule (Chemglass Life Sciences, part number CG-1880-31) equipped with a stirring bar, a thermocouple, and a pressure gauge. The ampoule was connected to a vacuum line and a PF The ampoule containing the starting material was evacuated to approximately 0.2 torr to remove nitrogen, and then 35 psig of PF 3 and heat the suspension under stirring. The contents are heated at a temperature range of 100°C-120°C under a PF of 20-35 psig. 3 for 4 hours, during which PF was added portionwise when the pressure approached 20 psig. 3. During the reaction, PtCl, which was initially insoluble in hexadecane, 2 and PF 3 complete reaction and formation of a compound soluble in hexadecane, which partially sublimed as colorless crystals on the cooler part of the apparatus. After 4 hours, heating was stopped and the reaction mixture was cooled to room temperature. 3 condensed back into the cylinder, and a portion of the crystals were separated from the solution and analyzed; a portion of the upper hexadecane solution was also 19 F NMR analysis of the crystals dissolved in pure, anhydrous hexadecane 19 F NMR (σCFCl 3, ppm): -36.4 (m, J(Pt-F) = 628 Hz, J(PF) = 1320 Hz, PtCl 2(PF 3) 2). Hexadecane upper layer solution 19 F NMR (σCFCl 3, ppm): -32.5 (d, J(PF) = 1405 Hz, PF 3), -36.4 (m, J(Pt-F) = 622 Hz, J(PF) = 1318 Hz, PtCl 2(PF 3) 2). FTIR of the crystal (pure solid on Golden Gate™ probe, resolution 4 cm -1): 417 (sh, w), 447 (sh, w), 461 (m), 483 (s), 507 (s), 518 (s), 531 (m), 551 (s), 901 (vs), 907 (sh), 933 (vs), 961 (s), 969 (w), 974 (m), 985 (w) DSC of crystals: 19.0°C (phase transition), 72.5°C (phase transition), 118.3°C (melting point). b) In hexadecane from PtCl 2(PF 3) x (x = 1, 2) Synthesis of Pt(PF 3) 4. The colorless crystals from a) were placed in the upper hexane solution, copper (2.22 g, 34.9 mmol) was added and an ampoule (150 mL HW pressure glassware) was connected to a vacuum line and a PF 200-1000 flask. 3. The ampoule containing the starting material was briefly evacuated to approximately 2 torr to remove nitrogen, and then 40 psig of PF 3 and the suspension was heated at a temperature range of 100°C-130°C for 4 hours under stirring. The reaction was carried out under a PF of 20-40 psig. 3, where PF is added portionwise as the pressure approaches 20 psig 3. After 4 hours, the heating was stopped, the reaction mixture was cooled to 35°C, and Pt(PF 3) 4. PF 3. Some solvent was condensed in a trap (made of stainless steel) cooled with liquid nitrogen under static vacuum. 3) 4 from PF 3 and residual hexadecane were purified by trap-to-trap distillation. Pt(PF 3) The yield of 4 was 1.25 g (32%, low yield due to partial PtCl 2(PF 3) 2 and the upper solution was used for analysis in a). Pure product Pt(PF 3) 4 of 19F NMR (σCFCl 3, ppm): -11.5 (m, J(PF) = 1301 Hz, Pt(PF 3) 4). Pure product 1 H NMR (σSiMe 4, ppm): 0.23 (t, J = 6.1 Hz, 71.7 mol.%, Me 2SiF 2), 0.90 and 1.32 (28.3 mol.%, hexadecane). Examples 3. Synthesis of Pt(PF) in glass ampoule using hexadecane solvent 3) 4. PtCl 2 (8.75 g, 32.9 mmol), Cu (18.25 g, 287.2 mmol), and hexadecane (30.95 g, 40 mL) were loaded into an ampoule (150 mL HW pressure glassware from Chemglass Life Sciences, part number CG-1880-31) equipped with a stirring bar, a thermocouple, and a pressure gauge. The ampoule was connected to a vacuum line and a PF The ampoule containing the starting material was evacuated to approximately 0.2 torr to remove nitrogen, and then 40 psig of PF 3 and heat the contents under stirring. The contents are heated at a temperature range of 110°C-120°C under a PF of 20-50 psig. 3 and stirred for 5.5 hours, during which PF was added portionwise when the pressure approached 20 psig. 3. During the reaction, PtCl is formed 2(PF 3) 2 crystals and then consumed, and at the end of the reaction the reaction mixture contained two immiscible liquids. After 5 hours and 30 minutes the heating was stopped, the reaction mixture was cooled to 41°C, and Pt(PF 3) 4. PF 3. Some solvent was condensed in a trap (made of stainless steel) cooled with liquid nitrogen under static vacuum. 3) 4 from PF 3 and residual hexadecane were purified by trap-to-trap distillation. Pt(PF 3) The yield of 4 was 79% (14.2 g). 19 F NMR (σCFCl 3, ppm): -11.5 (m, J(PF) = 1301 Hz, 99.40%, Pt(PF 3) 4), -34.4 (d, J(PF) = 1402 Hz, 0.36%, PF 3), -92.4 (d, J(PF) = 2035 Hz, 0.23%, POF 3), -166.0 (s, 0.007%, SiF 4). Pure sample 1 H NMR (σSiMe 4, ppm): 0.23 (t, J = 6.1 Hz, 67.4 mol.%, Me 2SiF 2), 0.90 and 1.32 (6.9 mol.%, hexadecane), 1.45 (d, J = 6.1 Hz, 25.8 mol.%, P(O i Pr) 3) By 1 H NMR was used to determine the organic content. The resonance intensity of the organic compound was lower than that of 0.09 g Pt(PF 3) 4 samples were dissolved in 0.76 g of 0.03% (0.228 mg, 0.0026 mmol) SiMe 4) C 6D 6. Therefore, Pt(PF 3) The total amount of 4 organic compounds is less than 80 ppm. Examples 4. Synthesis of Pt(PF) in glass ampoule using xylene solvent 3) 4. PtCl 2 (2.19 g, 8.2 mmol), Cu (4.69 g, 73.8 mmol), and xylene (16.1 g) were loaded into a 150 mL pressure glass ampoule (Chemglass Life Sciences, part number CG-1880-31) equipped with a stirring bar, a thermocouple, and a pressure gauge. The ampoule was connected to a vacuum line and a PF 3. The ampoule containing the starting material was briefly evacuated to approximately 3 torr to remove nitrogen, and then 40 psig of PF 3 and heat the contents under stirring. Heat the contents at a temperature range of 100°C-120°C at a PF of 20-40 psig. 3 and stirred for 4.5 hours, during which PF was added portionwise when the pressure approached 20 psig. 3. During the reaction, PtCl is formed 2(PF 3) 2 crystals and then consumed, and at the end of the reaction the reaction mixture contained two immiscible liquids. After 4 hours and 30 minutes the heating was stopped, the reaction mixture was cooled to 38°C, and Pt(PF 3) 4. PF 3. Some solvent was condensed in a trap (made of stainless steel) cooled with liquid nitrogen under static vacuum. 3) 4 from PF 3 and the residual solvent xylene were purified by trap-to-trap distillation. 3) The yield of 4 was 95% (4.3 g). 19 F NMR (σCFCl 3, ppm): -11.5 (m, J(PF) = 1301 Hz, 99.58%, Pt(PF 3) 4), -34.4 (d, J(PF) = 1402 Hz, 0.39%, PF 3), -92.4 (d, J(PF) = 2035 Hz, 0.03%, POF 3), -166.0 (s, 0.01%, SiF 4). % from integration. Pure sample 1 H NMR (σSiMe 4, ppm): 0.12 (t, J = 6.1 Hz, 0.7 mol.%, Me 2SiF 2), 1.11 (t) and 2.56 (q) (18.8 mol%, Et-C 6H 5), 2.05 (s) and 2.14 (s) (79.4 mol.%, xylene), 6.97 (m, aromatic protons), 12.46 (br, 1.0 mol.%, fluorophosphoric acid). 1 H NMR confirmed the residual solvent. 3) 4 The sample was dissolved in 0.80 g of 0.03% (0.24 mg, 0.0027 mmol) SiMe 4 C 6D 6 in. 1 H NMR (σSiMe 4, ppm): 0.00 (s, 6.28 mol.%, SiMe 4), 1.07 (t) and 2.39 (q) (18.64 mol%, Et-C 6H 5), 2.02 (s, 11.41 mol.%, xylene), 2.14 (s, 63.67 mol.%, xylene), 6.97 (m, aromatic protons). If we recalculate the mol% to wt.%, and calculate that the solution contains 0.24 mg of TMS, the total amount of organic compounds is 4.27 mg, corresponding to 88 mg of Pt(PF 3) 4.85 wt.% in the 4 sample. Examples 5. Pt(PF 3) 4. Shelf life Shelf life studies were conducted at room temperature over a period of 12 weeks. 3) 4 Store at room temperature in a volume of 50 cm 3 , a 316 alloy single-ended micro sample cylinder with a blind cap attached, and an electropolished stainless steel micro canister with a blind cap attached (V = 400 cm 3 ). When Pt(PF 3) Before 4, both containers were baked at approximately 150°C and 30-50 mTorr in vacuum. The pure liquid Pt (PF 3) 4 of 19 F and 1 H NMR spectrum, from 19 F and 1 H NMR spectroscopy monitoring of Pt(PF 3) 4 Determination of relative amounts of impurities. The results of the shelf life study were surface 2 in. [ surface 2] *Starting amount on Day 1. In all experiments within 12 weeks, Pt(PF 3) 4 The relative amounts of the impurities were almost similar. For the 316 SS steel ampoule, the deviation was higher. These results demonstrate that Pt(PF 3) 4. Stability over time. picture 4 series Pt(PF) was prepared in a 400 mL electropolished stainless steel micro-tank at room temperature. 3) 4. The determination and the relative amount of impurities over time. 3) 4 is intended for use as a precursor for Pt-containing membranes in microelectronic devices or in the catalyst industry. Comparative Examples 1. Prepared from K using the formula from Angew. Chem. Int. Ed. [German Applied Chemistry] 1965, 4, 521 and RU 2478576 C2. 2PtCl 6 Start to synthesize Pt(PF 3) 4 Pt(PF) was synthesized according to the recipe from Angew. Chem. Int. Ed. [German Applied Chemistry] 1965, 4, 521 and RU 2478576 C2. 3) 4 is shown below surface 3. The experiments were conducted using a commercially available high-pressure reactor from Parr Instrument Company (Series 4540, 600 mL, rated at 5000 psig, equipped with the standard impeller used in Experiments #10 and #12 and a U-shaped anchor stirrer designed to effectively stir the solids in b). The method of RU 2478576 C2 utilizes pure hydrogen and a drying step after reduction. If water removal from the system by scaling is ever possible, it requires expensive safety equipment and a long time. surface 3, #10 was performed using 149 µm copper powder (copper powder packaged under argon by the supplier and used as is). #11 and #12 were performed using 425 µm copper powder (99.5%, from Sigma-Aldrich). The reaction was carried out according to [Angew. Chem. Int. Ed. [German Applied Chemistry] 1965, 4, 521] from PtCl. 2 (#12, surface 3) Start of Pt(PF) 3) 4, where Cu was prepared from < 425 μm sized copper powder (99.5% from Sigma-Aldrich). Pt(PF 3) 4 (in #10-12) was formed in low to moderate yields. See also surface 3. Comparative Example on a commercially available standard device: a certain amount of starting material K 2PtCl 6. PtCl 2. Cu was loaded into the reactor in a glove box with oxygen and moisture < 0.5 ppm. The reactor was sealed, connected to a vacuum line, evacuated to less than 0.2 Torr, cooled to less than -79°C and the required amount of PF was added under stirring at low temperature. 3 was introduced into reactions #10 to #12. The reactor was then warmed to room temperature and further to 105°C - 130°C and the contents were placed in a PF 3 pressure for 24 hours. The reactor contents were then cooled to 35°C - 45°C, and a portion of the gas (approximately 25% - 35%) was introduced into a pre-vacuum trap (0.44 L, stainless steel) cooled with a dry ice-isopropanol mixture. The reactor was closed, the trap was kept open for approximately 10 minutes, and the non-condensable gas was then introduced into a second trap (6 L, aluminum) cooled with liquid nitrogen. If the gas passed through was cooled to below 0°C, the transfer line and valve were heated. PF in the 6 L Al trap After 3 partial condensation, apply vacuum to the 6 L Al trap to make the pressure in the trap below 1 Torr. Repeat the operation until all PF 3 and Pt(PF 3) 4 was stripped from the reactor and collected in two different traps. 3) 4 wells were reconnected to a separate pre-vacuum vessel (50 mL, stainless steel). 3) The precursor well of 4 was warmed to room temperature while the receiving vessel was cooled with liquid nitrogen and all the Pt(PF) was distilled in the receiving vessel under static vacuum. 3) 4. After distillation, the receiving vessel was warmed to room temperature and the residual PF 3 released by the scrubber. Pt(PF) 3) The yields of 4 showed low to moderate yields, although RU 2478576 C2 claims yields of 60%-95%. The Pt(PF) obtained from the RU 2478576 C2 formulation 3) The low to moderate yields of 4 may be due to the lack of solvent. 1 H. 19 F NMR, in all experiments Pt(PF 3) The purity of 4 is greater than 97.9%. As an example, the pure product from experiment b) 19 F NMR (σCFCl 3, ppm): -11.5 (m, J(PF) = 1302 Hz, 97.9%, Pt(PF 3) 4), -34.4 (d, J(PF) = 1402 Hz, 0.2%, PF 3), -92.4 (d, J(PF) = 2035 Hz, 2.0%, POF 3). [ surface 3] Examples 6. Hexadecane solvent was used to generate K 2PtCl 6 Start to synthesize Pt(PF 3) 4. K 2PtCl 6 (79.5 g, 0.16 mol), Cu (120.6 g, 1.9 mol), hexadecane (100 g) were loaded into a reactor (Parr Instrument Company, series 4540, 600 mL, rated at 5000 psig) in a glove box. The reactor was transferred and connected to a vacuum line, evacuated to less than 0.3 torr and cooled to less than -79°C, and 387 g (4.4 mol) of PF 3 was introduced into the reactor. The reactor was then warmed to room temperature, stirring was started, the reactor was further warmed to 120°C and the contents were placed in a PF 3 pressure for 22 hours. The reactor contents were then cooled to 35°C - 45°C, and a portion of the gas (approximately 25% - 35%) was introduced into a pre-vacuum trap (0.44 L, stainless steel) cooled with a dry ice-isopropanol mixture. The reactor was closed, the trap was kept open for approximately 10 minutes, and the non-condensable gas was then introduced into a second trap (6 L, aluminum) cooled with liquid nitrogen. If the gas passed through was cooled to below 0°C, the transfer line and valve were heated. PF in the 6 L Al trap After 3 partial condensation, apply vacuum to the 6 L Al trap to make the pressure in the trap below 1 Torr. Repeat the operation until all PF 3 and Pt(PF 3) 4 was stripped from the reactor and collected in two different traps. 3) 4 wells were reconnected to a separate pre-vacuum vessel (50 mL, stainless steel). 3) The precursor well of 4 was warmed to room temperature while the receiving vessel was cooled with liquid nitrogen and all the Pt(PF) was distilled in the receiving vessel under static vacuum. 3) 4. After distillation, the receiving vessel was warmed to room temperature and the residual PF 3 released by the scrubber. Pt(PF 3) The yield of 4 was 23.2 g. 2PtCl 6 is 25.9%. surface 4, which lists the two reactions in this example and the above comparative example 1 from K 2PtCl 6 starts with Pt(PF 3) 4. #13 is from the above comparative example 1 #11, and #14 is the result of this example. The two reactions were carried out at the same temperature and PF 3Under pressure. 19 Integration of F NMR spectra for determination of Pt(PF 3) 4 series 99.48%. Pure product from experiment b) 19 F NMR (σCFCl 3, ppm): -11.5 (m, J(PF) = 1302 Hz, 99.48%, Pt(PF 3) 4), -34.4 (d, J(PF) = 1402 Hz, 0.3%, PF 3), -92.4 (d, J(PF) = 2035 Hz, 0.2%, POF 3). [ surface 4] exist surface 3. Using PtCl The low yield of 2 may be due to inefficient mixing of the components, coating of the metal with metal chloride during the reaction, and other factors associated with starting a reaction from two different solids and gases. The solution can be converted from a solid-gas system to a solution-solid system to achieve better mixing of the components and more efficient interaction of the components dissolved in the liquid phase with the suspended metal powder. However, no solution-solid system has been reported to date because the solvent is expected to undergo a catalytic reaction with the Pt precursor or intermediate. Although the subject matter described herein may be described in the context of illustrative implementations for processing one or more computing application features / operations of a computing application having user interaction elements, the subject matter is not limited to such specific implementations. Rather, the techniques described herein may be applied to any suitable type of user interaction element execution management method, system, platform, and / or device. It should be understood that many additional changes in the details, materials, steps, and arrangements of parts described herein and illustrated to explain the essence of the invention may be made by those skilled in the art within the principles and scope of the invention as expressed in the appended claims. Therefore, the present invention is not intended to be limited to the specific embodiments shown in the examples and / or drawings above. Although embodiments of the present invention have been shown and described, modifications thereof may be made by those skilled in the art without departing from the spirit or teachings of the present invention. The embodiments described herein are intended to be illustrative and non-limiting. Many variations and modifications of the compositions and methods are possible and are within the scope of the present invention. Accordingly, the scope of protection is not limited to the embodiments described herein, but is limited only by the claims that follow, the scope of which shall include all equivalents of the subject matter of the claims. 11:Cu powder 12:PtCl 213:PF 314: solvent 15: container 16: reactor 17: pre-vacuum trap 18: Pt (PF 3) 4 wells 19: metal ampoule 20: PF 3 traps 101: pipeline 102: addition funnel 103: addition pipeline 104: drying process 105: pipeline 106: pipeline 107: pipeline 108: bypass 109: packaging 110: pipeline The foregoing and other aspects, features and advantages of the present invention, as well as the invention itself, may be more fully understood by reference to the following detailed description of the invention when considered in conjunction with the following drawings. The accompanying drawings are presented for illustration purposes only and are not intended to be limiting of the present invention, in which: [ picture 1] is an exemplary disclosed synthesis of Pt(PF 3) 4. Block diagram of the system; [ picture 2a] is an exemplary disclosure of the use of Pt(Hal) 2 (Hal = F, Cl, Br or I) to start the synthesis of Pt(PF 3) 4. Flowchart of the method; [ picture 2b] is an exemplary disclosure of the use of Pt(Hal) 2(PF 3) x (x = 1, 2; Hal = F, Cl, Br or I) to start the synthesis of Pt(PF 3) 4. Flowchart of the method; [ picture 3] PtCl 2(PF 3) 2 crystals and PtCl in phase 2(PF 3) 2. The upper layer of hexadecane solution of the stopped reaction mixture 19 F NMR spectrum; and [ picture 4] Pt(PF) in an electropolished stainless steel micro-can at room temperature 3) 4. Determination and graph of the relative amount of impurities changing with time. none 11:Cu powder 12:PtCl 2 13:PF 3 14:Solvent 15:Container 16: Reactor 17: Pre-vacuum trap 18:Pt(PF 3) 4 wells 19:Metal ampoule 20:PF 3 wells 101: Pipeline 102: Adding funnel 103: Add pipeline 104: Drying process 105: Pipeline 106: Pipeline 107: Pipeline 108: Bypass 109: Packaging 110: Pipeline
Claims
1. A method for synthesizing Pt(PF3)4 (CAS # 19529-53-4), the method comprising the steps of: forming a platinum precursor Pt(Hal)2, wherein Hal = F, Cl, Br or I, and a suspension of metal powder in a solvent; introducing excess PF3 into the suspension of Pt(Hal)2 and the metal powder; forming a soluble reaction intermediate Pt(Hal)2(PF3)x (where Hal = F, Cl, Br or I; x = 1, 2) in the solvent by reaction of PF3 and Pt(Hal)2 under reaction conditions; and forming Pt(PF3)4 in the solvent by reaction between Pt(Hal)2(PF3)x, the metal powder and the excess PF3.
2. The method as described in claim 1, further comprising the steps of: synthesizing the soluble reaction intermediate Pt(Hal)2(PF3)x (Hal = F, Cl, Br or I; x = 1, 2), wherein the synthesis step comprises the steps of: dispersing the platinum precursor Pt(Hal)2 in the solvent to form a suspension of Pt(Hal)2, wherein Hal = F, Cl, Br or I; introducing PF3 into the suspension of Pt(Hal)2; and forming a solution of the soluble reaction intermediate Pt(Hal)2(PF3)x (Hal = F, Cl, Br or I; x = 1, 2) in the solvent by the reaction of PF3 and Pt(Hal)2.
3. The method as described in claim 1, wherein, The platinum precursor Pt(Hal)2 is anhydrous.
4. The method as described in claim 1, wherein, The soluble reaction intermediate Pt(Hal)2(PF3)x (Hal = F, Cl, Br or I, x = 1, 2) is anhydrous.
5. The method as described in any one of claims 1 to 4, wherein, The reaction conditions include a reaction temperature below approximately 200°C.
6. The method as described in any one of claims 1 to 4, wherein, The reaction conditions include a reaction pressure of less than approximately 300 psig.
7. The method as described in any one of claims 1 to 4, wherein, The metal powder is copper, zinc, or aluminum powder.
8. The method as described in any one of claims 1 to 4, wherein, The metal powder has a particle size ranging from 200 to 900 micrometers.
9. The method as described in any one of claims 1 to 4, wherein, This solvent is an anhydrous solvent.
10. The method as described in any one of claims 1 to 4, wherein, This solvent has a boiling point above 150°C.
11. The method as described in any one of claims 1 to 4, wherein, The anhydrous solvent is selected from the following hydrocarbon solvents: oxygenated hydrocarbon solvents having the general formula (CnH2n+1)2O (n ≥ 1) and H3C(O(CH2)2)nOCH3 (n ≥ 1), aromatic hydrocarbon solvents having the general formula (CnH2n+1)xC6H6-x (x ≥ 1, n ≥ 1), or alkane solvents having the general formula CnH2n+2 (n ≥ 1).
12. The method as described in any one of claims 1 to 4, wherein, The yield of Pt(PF3)4 is in the range of approximately 70%-99.9%.
13. The method as described in any one of claims 1 to 4, wherein, After purification, the purity of Pt(PF3)4 is approximately 90 wt.%–99.9 wt.%.
14. A method for synthesizing Pt(PF3)4 (CAS # 19529-53-4), the method comprising the steps of: a) forming a suspension of platinum precursor Pt(Cl)2 in a solvent selected from xylene or hexadecane; b) introducing excess PF3 into the suspension of Pt(Cl)2 to form a solution of Pt(Cl)2(PF3)x (x = 1, 2) in the solvent by a reaction between PF3 and Pt(Cl)2; c) adding copper powder to the Pt(Cl)2(PF3)x (x = 1, 2) solution; and d) forming Pt(PF3)4 by a reaction between the copper powder, PF3 and Pt(Cl)2(PF3)x in the solvent at a PF3 pressure below about 300 psig and a reaction temperature below about 200°C; 15. The method as described in claim 14, wherein, The copper powder has a particle size ranging from 200 to 900 micrometers.
16. The method as described in claim 14, wherein, This solvent is an anhydrous solvent.
17. A method for synthesizing Pt(PF3)4 (CAS # 19529-53-4), the method comprising the steps of: a) forming a suspension of platinum precursor Pt(Hal)2, wherein Hal = F, Cl, Br or I, and metal powder in a solvent; b) introducing excess PF3 into the suspension of Pt(Hal)2 and the metal powder; and c) forming Pt(PF3)4 in the solvent by a reaction between Pt(Hal)2, the metal powder and the excess PF3 under reaction conditions.
18. The method as described in claim 17, further comprising the step of: forming a soluble reaction intermediate Pt(Hal)2(PF3)x (where Hal = F, Cl, Br or I; x = 1, 2) in the solvent by reacting PF3 and Pt(Hal)2.
19. The method as described in claim 18, wherein, The soluble reaction intermediates Pt(Hal)2(PF3)x and Pt(Hal)2 are anhydrous.
20. The method as described in claim 17, further comprising the step of: synthesizing the soluble reaction intermediate Pt(Hal)2(PF3)x (Hal = F, Cl, Br or I; x = 1, 2), wherein the synthesis step comprises the following steps: The platinum precursor Pt(Hal)2 is dispersed in the solvent to form a suspension of Pt(Hal)2; PF3 is introduced into the suspension of Pt(Hal)2; and a solution of the soluble reaction intermediate Pt(Hal)2(PF3)x (Hal = F, Cl, Br or I; x = 1, 2) in the solvent is formed by the reaction of PF3 and Pt(Hal)2.
21. The method as described in claim 20, wherein, The soluble reaction intermediate Pt(Hal)2(PF3)x and the platinum precursor Pt(Hal)2 are anhydrous.
22. The method as described in claim 17, wherein, The reaction conditions include a reaction temperature below approximately 200°C.
23. The method as described in claim 17, wherein, The reaction conditions include a reaction pressure of less than approximately 300 psig.
24. The method as described in any one of claims 17 to 21, wherein, The metal powder is copper, zinc, or aluminum powder.
25. The method as described in any one of claims 17 to 21, wherein, The metal powder has a particle size ranging from 200 to 900 micrometers.
26. The method as described in any one of claims 17 to 21, wherein, This solvent is an anhydrous solvent.
27. The method as described in any one of claims 17 to 21, wherein, This solvent has a boiling point above 150°C.
28. The method as described in any one of claims 17 to 21, wherein, The anhydrous solvent is selected from the following hydrocarbon solvents: oxygenated hydrocarbon solvents having the general formula (CnH2n+1)2O (n ≥ 1) and H3C(O(CH2)2)nOCH3 (n ≥ 1), aromatic hydrocarbon solvents having the general formula (CnH2n+1)xC6H6-x (x ≥ 1, n ≥ 1), or alkane solvents having the general formula CnH2n+2 (n ≥ 1).
29. The method as described in any one of claims 17 to 21, wherein, The yield of Pt(PF3)4 is in the range of approximately 70%-99.9%.
30. The method as described in any one of claims 17 to 21, wherein, After purification, the purity of Pt(PF3)4 is approximately 90 wt.%–99.9 wt.%.
Citation Information
Patent Citations
Film forming method and film forming material
JP2008231473A
Synthetic and purification methods for phosphaplatin compounds and uses thereof
TW201741326A
Purification of metals from mixtures thereof
US20040093986A1
