# US 10,480,070 B2 · Delivery container with flow distributor

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- Number: US 10,480,070 B2
- Document ID: US10480070B2
- Status: Granted
- Kind: B2
- Application number: 15/587,095
- Filed: 2017-05-04
- Published: 2017-11-16
- Granted: 2019-11-19
- Earliest claimed: 2016-05-12
- Assignees: Versum Materials US, LLC
- Applicants: Versum Materials US, LLC
- Inventors: Charles Michael Birtcher; James Patrick Nehlsen; Sergei Vladimirovich Ivanov; Thomas Andrew Steidl; Kai Kang; Wade Hampton Bailey, III
- Web page: https://patentgrep.com/patent/US10480070B2

## CPC

- C23C 16/4481: {by evaporation using carrier gas in contact with the source material (C23C16/4486 takes precedence)}
- B01B 1/005: {Evaporation for physical or chemical purposes; Evaporation apparatus therefor, e.g. evaporation of liquids for gas phase reactions}
- B01D 1/14: with heated gases or vapours {or liquids} in contact with the liquid
- B01J 4/002: {Nozzle-type elements (nozzle-type reactors B01J19/26)}
- B01J 4/004: {Sparger-type elements}
- C23C 16/4482: {by bubbling of carrier gas through liquid source material}
- C23C: COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL (making metal-coated products by extrusion B21C23/22; covering with metal by connecting pre-existing layers to articles, see the relevant places, e.g. B21D39/00, B23K; metallising of glass C03C; metallising mortars, concrete, artificial stone, ceramics or natural stone C04B41/00; enamelling of, or applying a vitreous layer to, metals C23D; treating metal surfaces or coating of metals by electrolysis or electrophoresis C25D; single-crystal film growth C30B; by metallising textiles D06M11/83; decorating textiles by locally metallising D06Q1/04)
- B01B: BOILING; BOILING APPARATUS {; EVAPORATION; EVAPORATION APPARATUS}
- B01D: SEPARATION (separating solids from solids by wet methods B03B, B03D; by pneumatic jigs or tables B03B; by other dry methods B07; magnetic or electrostatic separation of solid materials from solid materials or fluids, separation by high-voltage electric fields B03C; centrifuges, vortex apparatus B04; presses per se for squeezing-out liquid from liquid-containing material B30B9/02; treatment of water C02F, e.g. softening by ion-exchange C02F1/42; {arrangements of air intake cleaners in gas turbine plants F02C7/05} ; arrangements or mounting of filters in air-conditioning, air-humidification or ventilation F24F13/28)
- B01J: CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS

## Abstract

Described herein are delivery containers, systems and methods using same for providing improvements to precursor utilization in the containers for deposition process, as well as the cleaning and refilling of the containers. The containers are designed with structures which allow a carrier gas to be delivered from a flow distributor. The flow distributor comprises a plurality of small openings (jets) through which the carrier gas enters the precursor chamber and impinges upon the surface of the chemical precursors to produce a vapor.

## Claims

### Claim 1

A container for delivering a chemical precursor to a process tool, comprising:
a sidewall;
a base,
a lid having a flat surface,
an inlet tube,
a hollow flow distributor comprising a plurality of small openings as jets, and
an outlet passing through the lid;
wherein
the inlet tube passes through the lid and extended into the flow distributor, and is in fluid communication with the flow distributor,
the jets are facing the base at an angle ranging from 60 to 90 degrees to the lid,
each jet has an equivalent diameter ranging from 0.01 inches (0.025 cm) to 0.25 inches (0.64 cm); and
the hollow flow distributor has hollow bars and a hollow showerhead, the hollow showerhead is centered in the hollow flow distributor with the hollow bars extended from the hollow showerhead parallel to the lid, the hollow showerhead is in fluid communication with the hollow bars.

### Claim 2 (depends on 1)

The container of claim 1, wherein the container has a shape selected from the group consisting of cylindrical, rectangular cuboid, right cuboid, rectangular box, rectangular hexahedron, right rectangular prism, rectangular parallelepiped, and combinations thereof; and the hollow flow distributor has a cross section shape selected from the group consisting of tubular, circular, square, rectangular, and combinations thereof.

### Claim 3 (depends on 1)

The container of claim 1, wherein the hollow showerhead has a cross section shape selected from the group consisting of tubular, circular, square, rectangular, and combinations thereof.

### Claim 4 (depends on 1)

The container of claim 1, wherein the hollow bars have an inner equivalent diameter ranging from ⅛″ to 1″ and each jet on the hollow bars has an equivalent diameter ranging from 0.01 inches (0.025 cm) to 0.05 inches (0.125 cm).

### Claim 5 (depends on 1)

The container of claim 1, wherein the hollow flow distributor has 2 to 16 hollow bars having an inner equivalent diameter ranging from ⅛″ to 1″ and sealed on the sides, and each jet on the hollow bars has an equivalent diameter ranging from 0.01 inches (0.025 cm) to 0.05 inches (0.125 cm).

### Claim 6 (depends on 1)

The container of claim 1, wherein the hollow showerhead structure having a height of ⅛″ to 1″ with cross section area parallel to the lid ranging from 30% to 90% of cross section area of the container parallel to the lid, and each jet on the hollow showerhead has an equivalent diameter ranging from 0.01 inches (0.025 cm) to 0.05 inches (0.125 cm).

### Claim 7 (depends on 1)

The container of claim 1, wherein the hollow showerhead has a height of ⅛″ to 1″, the hollow bars have an inner equivalent diameter ranging from ⅛″ to 1″ and are sealed on the sides, and each jet on the flow distributor has an equivalent diameter ranging from 0.01 inches (0.025 cm) to 0.05 inches (0.125 cm).

### Claim 8

A system for delivering a chemical precursor to a process tool, comprising:
the chemical precursor selected from the group consisting of metal halides, metal β-diketonates, metal β-diketoesterates, metal β-ketoiminates, metal β-diiminates, metal alkyls, metal carbonyls, alkyl metal carbonyls, metal cyclopentadienyls, metal cyclopentadienyls carbonyls, metal pyrrolyls, metal imidazolyls, metal amidinates, metal alkoxides, and combinations thereof;
wherein
the metal is selected from the group consisting of Mg, Ca, Sr, Ba, Y, La, Ce, Sm, Tb, Er, Yb, Lu, Ti, Zr, Hf, Fe, Co, Ni, Ru, Ir, Rh, Cu, Al, Sn, Pb, Sb, Bi, Te, Cr, Mo Ta, and W;
a container containing the chemical precursor; comprising:
sidewall,
a base,
a lid having a flat surface,
an inlet tube,
a hollow flow distributor comprising a plurality of small openings as jets, and
an outlet passing through the lid;
wherein
the inlet tube passes through the lid and extended into the flow distributor, and is in fluid communication with the flow distributor,
the jets are facing the base at an angle ranging from 60 to 90 degrees to the lid,
tip of each jet is located with a distance of greater or equal to 0.5 inches from the chemical precursor the jet is facing,
each jet has an equivalent diameter ranging from 0.01 inches (0.025 cm) to 0.25 inches (0.64 cm); and
the hollow flow distributor has hollow bars and a hollow showerhead, the hollow showerhead is centered in the hollow flow distributor with the hollow bars extended from the hollow showerhead parallel to the lid, the hollow showerhead is in fluid communication with the hollow bars.

### Claim 9 (depends on 8)

The system of claim 8, wherein the chemical precursor is selected from the group consisting of tungsten hexachloride, tungsten pentachloride, tantalum pentachloride, molybdenum pentachloride, hafnium tetrachloride, zirconium tetrachloride, dicobalt hexacarbonyl tert-butylacetylene (CCTBA), cyclopentadienyltungsten tricarbonyl hydride (CpW(CO)3H)), bis(isopropylcyclopentadienyl) tungsten dihydride (iPrCp)2WH2, bis(alkylcyclopentadienyl) tungsten dihydride (RCp)WH2, Ni(II)N,N′-di-tertiary-butylamidinate (Ni(II)(tBu-AMD)2), Ni(II)N,N′-di-isopropylamidinate(Ni(II)(iPr-AMD)2), Ni(II)N,N′-di-ethylamidinate(Ni(II)(Et-AMD)2), Ni(II)N,N′-di-methylamidinate(Ni(II)(Me-AMD)2), Co(II)N,N′-di-tertiary-butylamidinate(Co(II)(tBu-AMD)2), Co(II)N,N′-di-isopropylamidinate(Co(II)(iPr-AMD)2), tetrakis(dimethylamido)hafnium (TDMAH), tert-butylimino-tris(diethylamino)tantalum (TBTDET), tert-butylimido-tris(methylethylamino)tantalum (TBTEMT), pentakis(dimethylamino)tantalum, bis(tert-butylimino)bis(dimethylamino)tungsten (BTBMW), bis(tert-butylimino)bis(diethylamino)tungsten, bis(tert-butylimino)bis(ethylmethylamino)tungsten, bis(2,2,6,6-tetramethyl-3,5-heptanedionato)strontium, and combinations thereof.

### Claim 10 (depends on 8)

The system of claim 8, wherein the chemical precursor is selected from the group consisting of tungsten pentachloride, dicobalt hexacarbonyl tert-butylacetylene (CCTBA), tantalum pentachloride, tungsten hexachloride, molybdenum pentachloride, pentakis(dimethylamino)tantalum, and combinations thereof.

### Claim 11 (depends on 8)

The system of claim 8, wherein the container has a shape selected from the group consisting of cylindrical, rectangular cuboid, right cuboid, rectangular box, rectangular hexahedron, right rectangular prism, rectangular parallelepiped, and combinations thereof; and the hollow flow distributor has a cross section shape selected from the group consisting of tubular, square, rectangular, and combinations thereof.

### Claim 12 (depends on 8)

The system of claim 8, wherein the hollow showerhead has a cross section shape selected from the group consisting of tubular, circular, square, rectangular, and combinations thereof.

### Claim 13 (depends on 8)

The system of claim 8, wherein
the hollow flow distributor has connected hollow bars and extended parallel to the lid, wherein the hollow bars have an inner equivalent diameter ranging from ⅛″ to 1″, and sealed on the sides;
each jet on the hollow bars has an equivalent diameter ranging from 0.01 inches (0.025 cm) to 0.05 inches (0.125 cm); and
the chemical precursor is selected from the group consisting of tungsten pentachloride, dicobalt hexacarbonyl tert-butylacetylene (CCTBA), tantalum pentachloride, tungsten hexachloride, molybdenum pentachloride, pentakis(dimethylamino)tantalum, and combinations thereof.

### Claim 14 (depends on 8)

The system of claim 8, wherein
the hollow showerhead having a height of ⅛″ to 1″ with a cross section shape selected from the group consisting of tubular, circular, square, rectangular, and combinations thereof;
the hollow showerhead has cross section area parallel to the lid ranging from 30% to 90% of cross section area of the container parallel to the lid, and
each jet on the hollow showerhead has an equivalent diameter ranging from 0.01 inches (0.025 cm) to 0.05 inches (0.125 cm), and
the chemical precursor is selected from the group consisting of tungsten pentachloride, dicobalt hexacarbonyl tert-butylacetylene (CCTBA), tantalum pentachloride, tungsten hexachloride, molybdenum pentachloride, pentakis(dimethylamino)tantalum, and combinations thereof.

### Claim 15 (depends on 8)

The system of claim 8,
wherein the hollow showerhead having a height of ⅛″ to 1″, the hollow bars have an inner equivalent diameter ranging from ⅛″ to 1″ and are sealed on the sides, and each jet on the flow distributor has an equivalent diameter ranging from 0.01 inches (0.025 cm) to 0.05 inches (0.125 cm); and
the chemical precursor is selected from the group consisting of tungsten pentachloride, dicobalt hexacarbonyl tert-butylacetylene (CCTBA), tantalum pentachloride, tungsten hexachloride, molybdenum pentachloride, pentakis(dimethylamino)tantalum, and combinations thereof.