METHOD FOR MAKING A PYROLYTIC BORON NITRIDE ARTICLE
A method for producing a pyrolytic boron nitride (PBN) article comprises introducing a nitrogen containing gas and a boron containing gas into a heated reactor furnace under temperature and pressure conditions sufficient to form a PBN deposit and pulsing the flow of the reactant gases between an on and an off state. The method provides a multi-layered PBN article that exhibits a relatively weak bonding interface between adjacent PBN layers to allow for the layers to be peeled away from one another in a controlled manner.
1 . A method of making a PBN article comprising:
introducing ammonia gas and a boron halide gas into a heated furnace reactor for a first period of time, reacting the ammonia and the boron halide and causing boron nitride to be deposited on a substrate;
after the first period of time, pulsing the flow of the ammonia gas and the boron halide gas into the reactor between a first pulsed state and a second pulsed state, the first pulsed state comprising discontinuing the flow of at least one of the ammonia gas and the boron halide gas, and the second pulsed state comprising flowing both the ammonia gas and the boron halide gas into the reactor and causing boron nitride to be deposited; and
pulsing between the first pulsed state and the second pulsed state until a PBN article of a desired thickness has been achieved.
2 . The method of claim 1 , wherein the first pulsed state comprises discontinuing the flow of both the ammonia gas and the boron halide gas.
3 . The method of claim 1 , wherein the first pulsed state comprises discontinuing the flow of the ammonia gas.
4 . The method of claim 1 , wherein the first pulsed state comprises discontinuing the flow of the boron halide gas.
5 . The method of claim 1 , wherein first pulsed state has a time interval of from about 0.5 to about 30 minutes.
6 . The method of claim 1 , wherein the first pulsed state has a time interval of from about 1 to about 15 minutes.
7 . The method of claim 1 , wherein the first pulsed state has a time interval of from about 5 to about 10 minutes.
8 . The method of claim 1 , wherein the second pulsed state has a time interval of from about 10 to about 150 minutes.
9 . The method of claim 1 , wherein the second pulsed stated has a time interval of about 90 to about 120 minutes.
10 . A method of forming a PBN article comprising:
(a) introducing ammonia gas and boron halide gas into a heated reactor furnace and reacting the gases for a first time interval to form a PBN deposit on a substrate;
(b) discontinuing a flow of the boron halide gas into the reactor for a second time interval; and
(c) repeating steps (a) and (b) until a PBN article of a desired thickness has been achieved.
11 . The method of claim 10 , wherein the first time interval is from about 10 to about 150 minutes.
12 . The method of claim 10 , wherein the first time interval is from about 90 to about 120 minutes.
13 . The method of claim 10 , wherein the second time interval is from about 0.5 to about 30 minutes.
14 . The method of claim 10 , wherein the second time interval is from about 1 to about 15 minutes.
15 . The method of claim 10 , wherein the first time interval is from about 90 to about 120 minutes, and the second time interval is from about 1 to about 5 minutes.
16 . The method of claim 15 , wherein step (b) further comprises discontinuing the flow of the ammonia gas during the second time interval.
17 . A PBN article made according to the method of claim 1 .
18 . A PBN article made according to the method of claim 10 .
19 . A PBN article comprising a plurality of PBN layers and a bonding interface layer disposed between adjacent PBN layers, wherein the bonding interface layer is substantially free of a dopant.
20 . A method of testing the peeling performance of a PBN article comprising:
subjecting a slab of a PBN article to ultrasonic forces for a period of time; and
determining the density of delamination between two or more PBN layers of the PBN article.