# US 11,111,256 B2 · High purity trisilylamine, methods of making, and use

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- Number: US 11,111,256 B2
- Document ID: US11111256B2
- Status: Granted
- Kind: B2
- Application number: 16/061,477
- Filed: 2016-12-16
- Published: 2020-08-20
- Granted: 2021-09-07
- Earliest claimed: 2016-12-16
- Assignees: Jiangsu Nata Opto-Electronic Materials Co. Ltd.
- Applicants: Jiangsu Nata Opto-Electronic Materials Co. Ltd.
- Inventors: Barry M. Ketola; Jesse A. Maddock; Brian D. Rekken; Michael D. Telgenhoff; Xiaobing Zhou
- Web page: https://patentgrep.com/patent/US11111256B2

## CPC

- C07F 7/10: containing nitrogen {having a Si-N linkage}
- B01J 31/146: {of boron}
- C01B 21/087: containing one or more hydrogen atoms
- C01B 33/027: by decomposition or reduction of gaseous or vaporised silicon compounds other than silica or silica-containing material
- C07F 7/025: {without C-silicon linkages}
- C07F 7/0803: {Compounds with Si-C or Si-Si linkages}
- C07F 7/20: Purification, separation
- C08G 77/62: Nitrogen atoms
- C23C 16/345: {Silicon nitride}
- C23C 16/45553: {characterized by the use of precursors specially adapted for ALD}
- H10P 14/6681: {the precursor containing a compound comprising Si}
- B01J 2231/005: General concepts, e.g. reviews, relating to methods of using catalyst systems, the concept being defined by a common method or theory, e.g. microwave heating or multiple stereoselectivity
- B01J 2531/002: Materials
- C07F: ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM (metal-containing porphyrins C07D487/22)
- B01J: CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- C01B: NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; {METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C}
- C08G: MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- 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)
- H10P: GENERIC PROCESSES OR APPARATUS FOR THE MANUFACTURE OR TREATMENT OF DEVICES COVERED BY CLASS H10

## Abstract

A composition, comprising: trisilylamine and less than 5 ppmw of halogen. A method of making a silylamine comprising combining ammonia and a compound comprising aminosilane functionality, where the compound comprising aminosilane functionality is according to formula (I) R1 N(R2)a(SiH3)2−a (I), where R1 is an organic polymer, a C-1-20 hydrocarbyl group or —SiR331, where R3 is C1-6 hydrocarbyl, R2 is a C-1-20 hydrocarbyl group, H, or —SiR331, where R3 is as defined above, subscript a is 0 or 1, provided that R1 and R2 may be the same or different except if R1 is phenyl, R2 is not phenyl, under sufficient conditions to cause a reaction to form a silylamine and a byproduct.

## Claims

### Claim 1

A method of making a silylamine, the method comprising: combining ammonia and a compound comprising aminosilane functionality, where the compound comprising aminosilane functionality is according to formula (I)
R1N(R2)a(SiH3)2−a (I),
where R1 is an organic polymer, a C1-20 hydrocarbyl group or —SiR33, where R3 is C1-6 hydrocarbyl, R2 is a C1-20 hydrocarbyl group, H, or —SiR331, where R3 is as defined above, subscript a is 0 or 1, provided that R1 and R2 may be the same or different except if R1 is phenyl, R2 is not phenyl,
under sufficient conditions to cause a reaction to form a silylamine and a byproduct; and
wherein the sufficient conditions include a temperature from −20° C. to 150° C. and a pressure greater than 102 kPa.

### Claim 2 (depends on 1)

A method according to claim 1 wherein the silylamine is trisilylamine, N(SiH3)3.

### Claim 3 (depends on 1)

A method as in claim 1, wherein the temperature is from 0° C. to 75° C.

### Claim 4 (depends on 1)

A method as in claim 1, wherein R1 is alkyl and each R2 is independently R1 or H.

### Claim 5 (depends on 4)

A method as in claim 4, wherein R1 is branched alkyl having 3 to 6 carbon atoms, and each R2 is independently R1 or H.

### Claim 6 (depends on 1)

A method according to claim 1, wherein the combining is in a pressure reactor.

### Claim 7 (depends on 1)

A method as in claim 1, wherein the pressure of the sufficient conditions is up to 300 kPa.

### Claim 8

A method of making a silylamine, the method comprising: combining ammonia and a compound comprising aminosilane functionality, wherein the compound comprising aminosilane functionality is an organic polymer comprising one or more groups according to formula (II)
—N(R2)a(H)b(SiH3)2−a−b (II)
where R2 is H, C1-20 hydrocarbyl, or —Si(R3)3, where R3 is C1-6 hydrocarbyl, subscript a and b independently are 0 or 1, and a+b<2, where the groups according to formula (II) are in pendant, terminal, or pendant and terminal positions on the organic polymer.