TW486392B - Solvent blend for use in high purity precursor removal - Google Patents

Abstract

The present invention is a process for cleaning a manifold which delivers high purity source chemical from a high purity source chemical container to a point of use after delivery of the high purity source chemical through the manifold is discontinued, comprising; evacuating the manifold by connection to a source of vacuum, terminating the evacuation, introducing at least one solvent for the high purity source chemical into the manifold from at least one source of the at least one solvent, dissolving any residual high purity source chemical in the manifold into the at least one solvent, venting a resulting mixture of residual high purity source chemical and solvent from the manifold, purging such as by pressurizing the manifold by connection to a source of preferably elevated pressure inert gas and terminating the purging i.e. pressurizing, before reintroducing high purity source chemical into the manifold.

Description

Background of the invention and other inventions where the invention is a needle-based solvent. The operation of the delivery pipeline can be successful without problems. The use of solvents to test ... It is necessary to be T% pure for the residues of chemicals or chemicals used for admixtures. So fast and effective for chemical cleaning of electrons. The method is to remove chemicals from pipelines efficiently. When the products in I industry are transported to the chemical industry, the special chemicals are evacuated and the vacuum volatile extraction is high. The delivery of the products is when the container is used for gas extraction and chemical toxic solvents and residual cleaning systems. It is not new here that the scope of chemical delivery is explicitly used. More specifically, when this pipeline, container and related chemical delivery pipelines are replaced. Washing has been used to remove both inert gas and cleaning, but for low-volatile chemicals, safety will be a 'there are some patents that try to make them fully listed. When participating in US Patent No. 5,045, 1 17 A method and a device for cleaning printed circuit assemblies by using a solvent and a vacuum are described. 1. A device and method for producing a semiconductor wafer by using an isopropanol solvent are disclosed in US Patent No. 5, 1 1 5, 576. ^ Additional patents related to solvent cleaning include: US Patent No. 5,744,436 5; US Patent No. 5,605,647; US Patent No. $ 494, 60 1; US Patent No. 5, 560, 86 1 US Patent No. 4, 578, 209; US Patent No. 5, 1 35, 676; US Patent No. 5 607, 91 2; US Patent No. 5, 762, 8 17; US Patent No. ' No. 5,352,375; U.S. Patent No. 5,827,454, U.S. Patent No. 5

486392 V. Description of the invention (2) 275,669; US Patent No. 5,75,0,488; US Patent No. 5,444,102; US Patent No. 6,040,749; US Patent No. 5,531,916; United States Patent No. 5, 1 1 8, 35 9; US Patent No. 5,298,083; US Patent No. 5304 322; US Patent No. 5 562, 86 1; US Patent No. 5, 685, 9 1 5; US Patent No. 5, 695, 688; US Patent No. 5, 71 6, 549; European Patent No. 710715A1; Japanese Patent No. 731 6595A2; Japanese Patent No. 8034996A2; Japanese Patent No. 8 j 2〇298A2. The invention innovatively uses a solvent blend (especially an all-hex / heptan joint) to overcome the previous cleaning operation of the pipe = point: it is super clean in cleaning-a chemical delivery system: the best cleaning Effect and minimal environmental impact .: High purity precursors in the carousel pipeline must be removed ^, in a 4b case, it has been formed early and the tongue removal is too low, in order to use: The volatility of the precursors in the delivery pipeline can be overcome by the previous: vacuum cleaning technology to remove it. The features and advantages of this invention are described in the following. The point will be to clean the manifold with a τ document in more detail. High-purity source chemicals are transported into the chemical container after being interrupted: the manifold is sent by a high-purity source = connected to a vacuum source :: Fang Ya stops emptying from at least one of the solvents ",, and One source will be at least-one soluble these high

Page 7 486392 V. Description of the invention (3) --------- The solvent of purity originating chem. Port 0 is introduced into the manifold, and any remaining high-purity ^ source chemicals in the manifold are dissolved in this at least one The solvent and the final mixture of residual high-purity source chemicals and solvent are discharged from the manifold. Preferably, after the solvent is discharged, it is connected to an inert gas source for flushing, and then the flushing work is ended. Optionally, the present invention can discharge the remaining chemicals from the manifold without prior evacuation and cleaning or pressurization 'just before solvent flushing. In this example, the present invention is a method for decontaminating a manifold after a high-purity source chemical is interrupted using a manifold to transport the high-purity source chemical to a used container. position. This method includes: connecting an outlet to empty the manifold, then terminating the emptying, and introducing at least one solvent soluble in the radon purity chemicals from the at least one source of at least one solvent into the manifold, and introducing the manifold In the tube! Any residual high-purity source chemical is dissolved in this at least one solvent | and the final mixture i of this residual high-purity source chemical and solvent is discharged from the manifold. Preferably, such at least one solvent is a fluorocarbon-containing solvent and a hydrocarbon > cereal. More desirably, the at least one solvent is a blend of a solvent and a solvent which renders the high purity source chemical nonflammable. Most desirably, the at least one solvent is a blend of a solvent and a solvent that renders the high-purity source chemical non-hazardous. This high-purity chemical is selected from the group consisting of: pentaethyl oxide button (ΤΑΕΤΟ), tetrakis (diethylamino) titanium (TDEAT), tetrakis (dimethyl)

486392 V. Description of the invention (4) Amine-based titanium (TDMAT), tetramethylcyclotetrasiloxane · fired (TMCTS), copper hexafluoroacetamidinepyruvate-trimethylvinylsilane ((: 11 (1 ^ & (:: ^^^ 5), Tetraethylorthoquatate (TEOS), Trimethylborate (TMB), Triethylborate (TEB), Triacetite (TMPi), Triethyl phosphate Esters (TEPO), bis-tertiary-butylaminostilbane (BTBAS), tantalum ethoxylate dimethylaminoethoxylate (TAT-DMAE), tertiary-butyliminotridiethylamine button ( TBTDET), triethyl arsenite (TEOA), polyaryl ethers, and mixtures thereof. This at least one solvent is selected from the group consisting of: organic alcohols (such as methanol, ethanol, propanol, butanol) , Propylene, Tetrahydropyrene, Dimethyl sulfide, Water, Aliphatic hydrocarbons (such as hexane, heptane, scorch, decant and twelve), aromatic hydrocarbons, ketones Types, disks, hydrocarbons, ethers, esters, glyces, aromatic hydrocarbons, halogen-containing alcohols, alkyl nitriles, organic amines, fluorinated compounds, fully-fluorinated carbon compounds (such as And perfluorinated heptane) and mixtures thereof. DETAILED DESCRIPTION OF THE INVENTION The present invention includes a method using a solvent with a low purity and low nuclear impact, which can be used in chemical vapor deposition (CVD) and other semi- " conductors The manufacturing procedure contains a solvent flushing procedure for the inner surface of a high-purity working pipeline containing residual ultra-high purity and precursors with low vapor pressure. The present invention can be used in US Patent No. 5,964,230 (as of October 1, 1999) It was transferred to the applicant of this case on the 2nd), which is specially added here for reference.

486392 V. Description of the invention ⑸-, standard vacuum cycle flushing is removed from the inside of the high-purity operation pipeline system. The results of incomplete removal include safety hazards to the operator, and the precursor's reactivity to air and moisture may form particles and cause pollution. Response, or even a more aggressive response. For these substances, the solvents with the best solubility are usually hydrocarbons and / or chlorofluorocarbons (CFCs), which are flammable, toxic, corrosive, reactive, or have adverse environmental effects. In the case of ethanol, it has national and international restrictions on additional shipping. In addition, because these precursor materials are usually sensitive to air and / or moisture, they need to be removed from the inner wall of the work line as much as possible. '”For the purposes of the present invention, hazardous generational sounds σ = academic precursors are those that meet the standards of government agencies (such as the US Environmental Protection Agency 2 ，, as in Barc 1 ay s California regulations, The 22nd question is set out in Nos. 66261.30- 6 6 261.33. In the past few years, many cleaning solvents have been identified for cleaning the residues of some projects, from printed circuit boards to automobiles. The dynamics of the body are diversified. In these examples, the removed material is an unwanted product, not an ultra-pure precursor in the operating chemical delivery pipeline, and the * 刎 pipeline must maintain ultra-high purity. 14 Some * While trying many compounds, the inventor has found in the current literature a method and a suitable solvent or solvent blend. &Amp; A

It is aimed at the use of blended solvents and pure solvents, which meets the safety, method and environmental requirements of semiconductor industry, health and regional regulations. 3 The preferred blends include 'all-I carbon compounds ( As a carrier solvent, in some cases as the main solvent) and with appropriate solubility, vapor ^ 486392

And flash point hydrocarbon solvents. Pure substances should include all kinds of non-combustible or flammable alcohols, ethers, acetone and other polar and non-polar solvents, and their mixtures. Two of them can be mixed with each other, and also with inert carrier solvents. Phase mixing. In addition, supercritical fluids (such as liquid carbon dioxide) can be considered. 1㈣ A more specific example of the use of a solvent flushing device in U.S. Patent No. 5, 9 6 4, 2 3 0 is: most of the precursors of the process chemicals are inert gases (helium | nitrogen, argon or other suitable Inert gas) is flushed from the area of the operation pipeline that needs to be flushed, leaving only the 7 ^ operating chemical precursors stuck to the pipe wall. In the case of hydrogenated substances, the dissolution of the repellent was observed in the adjuvant system. Absorptivity and anti-energy determine the quality of any purely contaminated substance consisting of a solvent and a solvent—reserving one 丨 ___ one 1 ... adjuvant mediation, local hexane or or A single amount to be flushed, and as an alternative, it can contain the inlet inlet and the solvent to be evacuated. Areas of similar substances and carbon unblended solvents. Among them, the previous solvent can be easily removed. A kind of carbon or other inhaled mixture of a depleting agent must be tested before washing the internal carrier of the device to be rinsed in the perfluorinated carrier (eg, hexane, heptane). The solvent is injected under pressure under pressure. Dissolved substances that meet safety and environmental requirements can be used. The solvent will be introduced into a color-resistant. Sen's or Neptune's choice of a precursor and this kind of precursor toxicity and corrosiveness are directly coated with solvents to clean the pipeline ^ ^ 深 幻 円 # Until all precursors are gone.

Agent cleaning is described further below. The initial solitary tongue L is filled with a suitable solvent and cleaning method. The month, no clothes% & Road can be removed quickly and completely.

11 Page 11 486392 V. Description of the invention (7) Operating chemicals, such operating chemicals or high-purity source chemicals include (but not limited to): pentaethoxylate (TAETO), tetrakis (diethylamino) ) Titanium (TDEAT) 'tetrakis (dimethylamino) pyridine (TDMAT), hexafluoroethyl-propionate-acid steel-trimethylvinylsilane (Cu (hf ac) TMVS) and similar chemical vapor deposition copper precursors Materials, tetraethyl orthosilicate (TEOS) and other chemical vapor deposition (CVD) silicon precursors [such as tetramethylcyclotetrasiloxane (TMCTS), CVD precursors containing butterfly and phosphorus (such as triborate Tetramethyl ester (TMB), triethyl borate (TEB), trimethyl phosphite (TMpi), triethyl phosphate (TEp0)), bis second butylamino sulfonyl phosphate (BTBAS), tetraethoxy group Diamidinoaminoethoxylate (TAT-DMAE), tertiary butyliminotridiethylamine button (TBTDET), triethylarsenate (TEASAT) and similar arsenic precursors [eg arsenite Diethyl ester (TEOA)], low-K spin-coating substances (e.g.

Polyarylether VELOX obtained by Air Products and Chemicals, fluorinated aryl FLARE obtained from Honelwel 丨, Michigan, USA, aromatic hydrocarbons obtained from Dow Chemical 0f, Michigan, USA Resin SILK) and other related compounds. Basically, the solvents considered in the present invention include organic alcohols (e.g., methanol, ethanol, propanol, butanol), acetone, and tetrachloroarsine. South: methyl alcohol, water, aliphatic hydrocarbons (such as hexane and undecane), aromatic hydrocarbons, classes, aldehydes: substances, ethers, vinegars, glyces, aromatic dishes Hydrogen compounds, containing

Li alkane, alkyl alcohol, organic amine, ☆ fluorinated compound, perfluorocarbon δ, perfluorinated hexane, perfluorinated heptane and mixtures thereof. Hydrocarbons are the preferred main solvents, such as petroleum and agricultural raw materials. 486392 V. Derivatives of Invention Note (8); Alcohols; Glycols; Glycol ethers; G-classes; Aldehydes; Ketones Ethers; autogen-containing hydrocarbons; nitrogen-containing compounds; sulfur-containing compounds; silicon-containing compounds; n-heptane; 2- and 3-fluorenyl hexane; 2, 3-and 3, 3-dimethylpentyl Burning; 2,4- and 2,2-difluorenylhexane; dimethylcyclopentane; methylcyclohexyl: and ethylpentane. Other hydrocarbons can also be considered, such as n-fluorene; 2-methylbutane; 2,2-difluorenylpropane; n-hexane; 3-fluorenylpentane; 2,2-difluorenylbutane ; 2,3-Difluorenylbutane; n-heptane; 2-methylhexane; 3-methylhexane; 2, 3-difluorenylpentane; 2, 4-difluorenylpentane; n Octane; 2, 2, 3-trimethylpentane; 2, 2, 4-trimethylpentane; cyclopentane; cyclohexane; fluorenyl cyclohexane; ethyl cyclohexane; carbon chloride Hydrogen compounds (such as dichloromethane and cis-dichloroethylene). Aromatic, carbonyl-containing, halogen-containing, and oxygen-containing solvents can also be considered, for example: trans-1,2-dichloroethylene, trichloroethylene, and tetrakiethylene; ketones (such as acetone, fluorenyl ethyl ketone, Fluorenyl butyl ketone and fluorenyl isobutyl ketone ethers (such as diethyl ether, fluorenyl-2-ethoxyethanol, tetrahydrofuran and 1,4-dioxane); fluorochlorohydrocarbons (Such as 2,2-dichloro ~ 1,1, 丨 ―trifluoroethane and 1,1_dichloro-1 -fluoroethane); esters (such as methyl acetate, ethyl acetate, propyl acetate, and Butyl acetate); nitrogen compounds (such as wall methane, nitroethane, nitropropane, and nitrobenzene); amines (such as diethylamine, triethylamine, isopropylamine, n-butyl Methylamine and iso-butylamine);% classification (such as phenol, o-cresol, m-cresol, p-cresol, thyme, p-third butyl phenol, third butyl catechin , Cat t echo 1, isobutanol, o-methoxyphenol, bisphenol A, isoamyl salicylate, stearic acid salicylate, methyl salicylate and 2, 6-di-tert-butyl -P-cresol) and triazole [for example 2 a (2,-

Page 13 486392 V. Description of the invention (9) 1-yl-5, -methylphenyl) benzothiazole, 2- (2,1-hydroxymeta-methylphenyl) -5-air benzothiazole, 丨2: 1 ^ double ~ 2-r glutamate,-* I 2, 3-benzothiazole and bu [(N, group α-ylhexyl) aminomethyl] benthiazole] and selected from the following families Alcohols composed of: butanol, 2 ~ ^^ free of the following group alcohols, 2-fluorenyl-2-propanol, pentyl alcohol, 2-1, 2 \ fluorenyl-1-propanol; vinegar; selected from the group consisting of V-butanol and 2-propanedipropane Λ composed of the following groups: pentane, 2,4: dimethylpentane, 2, 2- τ-propane, heptane, isobutane, hexane , 3-methylpentan, nonan,:;, 2-methylbutan, 3-methane, turpentine, and undecane. Where pentane, terpineol, propane or less flammability or environmental hazards, it hexane, tetrafluoromethane, m, 2, 2_ five: butane propane, tetrakis-pentane, 2-methyl 2-tetrafluorobutane, 1, ii 2 2 3 3-membered difluoromethyl-1,1,1, heptafluorohexane, 2-monofluorofluoropentane, H, 1,2,2,3 , 3 a wide-cap '2 gas methyl-M ,. ~ Burn 1,2,2,3,3-Heptafluoropentane, 3 A for one buckle, Jade, Dingyuan, 1,1,1,2,2,3,3,4,4 ~ = Hexadiene / methyl 9yl ^ 1,1,2-tetrafluoro-^^ one "-hexafluoropentane ^^ pyridine ^ pyridinemethyl-per-butane, 1,1,1,2,2 , 3-hexafluoro-3 ~ three gas and formazan :, methyl-1, i, 1-trifluoroLL 1, 2, 2, 3, 3, 4, 4-nonafluoroheptane, 5 ~ earthane, 1 3,3,4,4-nonafluorohexane, 3-hexafluorohexane, 4-fluorenyl-2-trisgasamidine dimuridine-1, l I 2, 3, both methyl ~ 1 , 1,1,2,3,3-hexafluoropentane

486392 V. Description of the invention (ίο) $, 2 2; Di '曱]] ,!' Bu Sandun pent yaki, 3_ 曱 keto_2, 2_ trifluoromethyl,-, butyl yaki, ^, ^^ 6 Fluoro ^ trifluoromethylhexyl

Hyun 1,1,1,1,2,2,3-Six minutes one q one one speaks about Gan A, three random two fluorenyl-4-methylpentane, two trifluoro: yl--random Propylene, smut, tetrafluorobutyrate, 3_fluorenyl-// 乂 ^ 六六 乱 '烧 "-fluorenyl-1,1,1,2,2,3,3,4 ,, ^ 7 土 _ _Difluorofluorenyl-1, I 1,2,3-pentafluoropentane, 2-methyl-1,1,1, ^ 3 3 4,4 4- ^ aT ^ .3 ^^-1, ^ ^ 2,2,4,4,5, & Ten rats, 2_ fluorenyl-1,1,1,3,3,4, 4,5,5,5-decafluoropenta]], 'Tri Λ i / '1,2,2,4,4,5,5,5 ^^^, 2-^-1, 1 2 1: 3 3 4';, 5, 5 5_ Decafluoropentazol, 3_ Trifluoromethyl Yl 1 ι ι ι 2, 2_Hyun, 3_pentafluoroethyl pentafluorine, 4-trifluoromethane,-', 1,2: 2'3,3-heptafluorohexane, 2_methyl_ 2-trifluoromethyl butane, 2-methyl n; J '' air methyl-3,3,4,4,4-pentafluoro!】 彳 9 9 / Γ group, ^ 1-trifluorobutane , 3,3_dimethyl '' '2'2,4,4'5'5'5-decafluoropentane, 3_fluorenyl_3_trifluoromethyl_1'1'1'2, 2-pentafluoropentane, 3,3_bis (trifluoromethyl) pentane, 2,2_dioxine 1,1,1,3, 3, 4, 4, 5, 5, 5 -decafluoro Pentane, 2-methyl-2-trifluoromethyl-1,1,1-trifluoropentane It is true that working chemicals that are reactive but provide soluble by-products are also applicable to the present invention. For the purposes of the present invention, the term solvent is considered a broadly defined solvent. The types of "reactive" solvents include acids , Alkali and reactive solvents. Specific examples are: When ethanol * TDEAT is used together, the titanium oxide produced will be dissolved in ethanol to ensure complete removal. The use of nitric acid solution can be used to remove copper oxidation byproducts, while HF solution can be used

Page 15 486392 V. Description of the invention (11), " ~ '~ ------- Oxidation by-product substances such as titanium oxide or oxidation species. This kind of solvent with Γ 舻 ^ source chemical M " is broadly regarded as a considerable amount of sourced dimethyl t or base, and they play a role in dissolving high purity source chemicals with others, or with high purity sources. Chemicals react to form highly soluble fields. They may include HF, HN03, HC1, H2S04, NaOH, KOH, and other different oxidizing and / or reducing agents. They also act as organic acids and bases suitable for negative reactions with or removal of such permeants. In addition, after being mixed together in the manifold, this solvent may make the high-purity chemical no inert or at least become non-flammable. It can push fluorine and all organic or hydrocarbon liquids will be classified here = Solvent. Perfluorinated carbon compounds (such as perfluorinated hexane, perfluorinated heptane, and mixtures thereof) are examples of such solvents. In addition, inert compounds such as vacuum pump oils and / or similar low-volatile hydrocarbon or fluorocarbon oils can be used. Perfluorinated hexane is considered as a carrier solvent. It must keep a minimum of water content and dissolved oxygen ’to remove water and oxygen from perfluorinated carbon compounds. In this article, many perfluorocarbon compounds can be selected for use, but they must meet general guidelines: non-flammable or easily formed non-flammable, compatible with major solvents, non-reactive with precursors, easy to recycle or recycle, and Does not harm the environment. The choice of this primary solvent must have the following functions: it has the ability to absorb or dissolve the precursor, it must be more volatile than the vacuum provided, and it must have a consistent high flash point. These conditions may This will vary with different precursors and will require different primary solvents for this procedure. example

Page 16 486392 V. Description of the invention (12) ~ For example, TDMAT and TDEAT use hexane or heptane as the main solvent. Copper < ^ 1) precursors [eg (: 11 (11 £ 80〇1: 11 ^ 3) use trifluorene vinyl sulfite (TMVS) as the main solvent. This solvent substance is selected to remove various precursors Precursors include (but are not necessarily limited to) the group's precursors (such as TAETO and TBTDET), titanium precursors (such as TDEAT and TDMAT), copper precursors [including Cu (hfac) tmvs and any other copper-containing precursors] ( The olefin group can be used as a solvent, and the precursors of barium / strontium / titanium (BST) (they are usually solid themselves, and the carrier of various precursors for various solvents. Examples of precursors include Ba (thd) x, Sr (thd) x and Ti (thd) x). These technologies can also be used to flush out the arsenic compounds (such as TEAS AT and TE0A) in high-purity operation pipelines. Germanium, thorium, pins and other related Liquid precursors can also be removed using this technique and suitable dissolving reagents, depending on: the compound used. I The main solvent usually has a part of the compounds in the precursor molecule. Other precursors still use alcohols (such as ethanol , Isopropanol or methanol) as the main solvent. In all In the example, the main problem is the solubility of the precursor and the non-reactivity of this solvent with the carrier solvent. Examples of the main solvents used with TDMAT are hexane and heptane. I The operating limit of these solvents is based on the boiling point of these solvent mixtures And the flash point and the viscosity and phase of the precursor. The acceptable temperature range is the highest; it can be as low as 80 ° C or it can be reduced to about 0Ό, depending on the solvent and the precursor. 丨 Flushing gas or solvent delivery pressure range Preferably between 5 psig and 70 psig: However, unpressurized inert gas delivery is also considered. So for the purposes of the present invention, flushing is considered to be by using a vacuum in the manifold f

486392 V. Description of the invention (13) The weight ratio of inertia below atmospheric pressure or using an elevated pressure source and preferably emptying should be lower than the weight ratio of the two related blends. The amount is 10 weights. Use this solution to empty and rinse, remove before the source chemicals, only the residual drive is completely removed. The present invention is a method for carrying out the cleaning of ambiguous source chemicals, including: Purity-derived high-purity sources Retain high-purity sources, inert gas sources such as atmospheric pressure or super-atmospheric pressure, which are introduced into the manifold. Pressurization is considered the use of an elevated gas, where the pressure is at least raised to a superatmospheric pressure than the conditions under which it is evacuated. To ensure complete removal, the vapor pressure of the true solvent required. The range of the main solvent in the second or fluorinated solvent is preferably between 1% and 20%. The choice of blending is based on the flammability, the solubility of the precursor in the solvent, and the number of this period. . In a preferred embodiment, the amount of heptane is% 'and the rest is perfluorinated hexane. The solvent cleaning method combined with inert pressurized gas for traditional drainage can remove about 65% to 95% of the flooding substance after the first cleaning. The remaining part is almost completely reduced after the second cycle. After the third solvent rinse step, remove it. In some cases, additional cleaning was used to determine this. In this example, a lower concentration of solvent was used. Contains a method for interrupting a tube when using a manifold to deliver high-purity source chemicals, where the manifold is used to transport high-purity source chemicals to the location of use. This is connected to a vacuum source to evacuate the manifold, and then terminate at least one source of the seeding solvent. At least one solvent soluble in these chemicals is introduced into the manifold, and any residual chemicals in the manifold are dissolved in the at least one The solvent and the final mixture of residual chemicals and solvent are discharged from the manifold.

Page 18

Description of the Invention (After the IQ is released, the ㉟ method is then connected to the inert connection of the desired pressure to pressurize the manifold for flushing, and then finish the flushing work or the desired pressurizing work. Most jealous Working methods such as t Γ, dissolution, discharge and rinsing, or desired pressurization:% sequence is repeated repeatedly, and this is repeated one after another / times: ': Repeated twice: Cyclic After repeating the sequence, it is best to work with chemicals or high-purity source precursors into the manifold or 11th, and then empty and flush, or better pressurize the manifold. In the example, the emptying and flushing or preferably pressurizing the manifold is best ended by emptying the manifold, and the degree of emptying should be lower than the therapeutic pressure of the solvent blend. The present invention can avoid the previous emptying, but only discharge the residual chemicals from the manifold before washing with the solvent t. In this example, the month t Θ after the interruption of using the manifold to transport two purity source chemicals A method carried out to clear, where the manifold is composed of a high-purity chemical σσ Conveying high-purity source chemicals to a dumping position. This method includes: • Evacuating the manifold connected to an outlet, and removing at least one solvent that is soluble in these high-purity source chemicals from at least one source of at least one solvent. Into the manifold, dissolve any residual high-purity source chemicals in the manifold in at least one solvent, and discharge the final mixture of such residual high-purity source chemicals and solvents from the manifold. Specific examples of solvent blends are: The range of blending is that the amount of heptane is about 1% to 20% by weight, which is perfluorinated.

486392 Description of the invention (15) Pentane, a better ratio is that heptane accounts for 10% by weight, and the rest is perfluoro. The invention is used in a high-purity conveying system (14 :), which can provide significant advantages in maintaining the high purity of the source chemical. It is not only the purity of the source chemical, but also the emptying and cleaning of the chemical. In order to maintain the true quality of the 3-rings of the carousel system ... this kind of cyclic, green solvent is a solvent for low volatility and low volatility chemicals. To make; = 2 need to be suitable for this kind of t, the present invention does not affect 1 ;; == electricity 2 manufacturing agent and its disposal provides a way to dissolve this kind of: (Provided chemicals) provide super cleanliness including the problems existing in the source pipeline in the operation pipeline 'these problems are in the container and the same rotation m =, the durability and replacement of the source of the invention. The present invention has proposed different sources The scope of "Chemicals" should be applied by the following patent applications, but all the 486392 drawings of the present invention are briefly explained.

I Page 21

Claims (1)

486392 6. Scope of patent application1. A method for cleaning the manifold when the use of a manifold to transport high-purity source chemicals is interrupted, wherein the manifold transports the high-purity source chemicals to a place of use from a high-purity source chemical container The method includes connecting a vacuum source to empty the manifold, then terminating the emptying and introducing at least one solvent soluble in the high-purity source chemical into the manifold, the at least one solvent At least one source is derived, dissolving any residual high-purity source chemicals in the manifold in the at least one solvent, and draining the final mixture of residual high-purity source chemicals and solvents from the manifold, and then with a A source of inert gas is connected to flush the manifold. 2. The method according to item 1 of the scope of patent application, wherein the evacuation, introduction / dissolution and flushing are repeated in a cyclic sequence. 3 · If the method in the scope of patent application for item 2 is used, Zhizhong will evacuate and flush the manifold after repeating the process? According to the sequence, the method of the third item in the patent scope is requested, wherein the emptying and flushing of the manifold ends with emptying the manifold. Parallel and / f 冼 5 · If the scope of the patent application, agent j is a fluorocarbon. The method according to claim 1, wherein the at least one solvent is as per the scope of the patent application 是 r is a perfluorocarbon. Item of the method, wherein the fluorocarbon 486392 VI. Application for Patent Scope 7 · The method according to item 1 of the patent application scope, wherein the at least one solvent is a blend of a fluorocarbon-containing solvent and a hydrocarbon solvent 0 8 The method according to item 1, wherein the high-purity source chemical is selected from the group consisting of: tantalum pentaethoxide (TAETO), tetrakis (diethylamino) titanium (TDEAT), tetrakis (diethylamino) titanium (TDMAT), Tetramethylcyclotetrasiloxane 丨 | (TMCTS), copper hexafluoroacetamidinepyruvate-trimethylethylenesilane j (Cu (hfac) TMVS), tetraethyl orthosilicate (TE〇s), boric acid Trimethyl ester (TMB), triethyl borate (TEB), trimethyl phosphite (TMPi), triethyl phosphate (TEPO), bis third butylaminosilane (BTBAS), tetraethoxy button ; | Difluorenylaminoethoxylate (TAT-DMAE), tertiary butyliminotridiethylene: | ylamino group (TBTDET), triethylarsenite (TEOA), polyaryl ether and The group of its mixture. Day II.9. The method according to item 1 of the patent application, wherein the at least one solvent is selected from the group consisting of organic alcohols, such as methanol, ethanol, propanol, and butanol, propionate, tetrahydrofuran, Methylsiloxane, water, aliphatic hydrocarbons, such as hexane; heptane, octane, decane and dodecane, aromatic hydrocarbons; similar preparations, hydrocarbons, and bonds酉 类 类, g 1 ymes' fragrant 丨 丨 fragrant hydrogen compounds, containing alkanols, alkyl nitriles, organic amines, fluorinated λ. / LjLj inlet, king fluorinated carbon compounds, such as perfluorinated A group of hexane and perfluorinated heptane, and | mixtures thereof. Page 23 VI. Scope of patent application, " " -------------- Clean the 1 manifold: = Profit: ί: ?? High-purity source chemicals will be cleared after interruption Following the ancient method, the eighth delta kiwi officer is operated by a high-purity chemical source = purity-source chemical to the place of use. The method includes: ····························· The connection is used to empty the manifold. Then, the evacuation is terminated, and a solvent of perfluorinated hexane and heptane of a high-purity source chemical is dissolved from a diluent + source. The solvent blend is introduced into the manifold, and Dissolve any residual chemicals in the solvent from the source to the purity, and dissolve the residual chemicals, and the final mixture of source chemicals and solvents, out of the manifold. Connect to flush the manifold. 11. The method according to item 10 of the patent application range, wherein the solvent is blended; the weight proportion of heptane in the content is about 1% to 20%, and the remaining is fluorinated hexane. Wang I 12. The method according to item 10 of the scope of patent application, wherein the weight ratio of heptane in the solvent exchange is about 6%, and the rest is perfluorinated. 13 | A method of cleaning the manifold when the use of a manifold to deliver high-purity source chemicals is discontinued || The manifold is used to transport high-purity source chemicals to a used container from a high-purity source chemical I container Position, the method includes ... connecting to an outlet to empty the manifold, then terminating the emptying and introducing at least one j-soluble solvent into the manifold, the at least Page 24 486392 VI. Scope of patent application A solvent is derived from at least one source. Any remaining high-purity source chemicals in the manifold are dissolved in the at least one solvent, and the remaining high-purity source chemicals and solvents are finally The mixture is discharged from the manifold. 14. The method of claim 13 in the scope of patent application, wherein the at least one solvent is a fluorocarbon t * compound. 15. The method of claim 14 in which the fluorocarbon is a perfluorinated hydrocarbon. 16. The method of claim 13 in the scope of patent application, wherein the at least one solvent is a blend of a fluorocarbon-containing solvent and a hydrocarbon solvent. Page 25