# US 2021/0277500 A1 · Method for preparing single crystal superalloy test bars by using ni-w heterogeneous seed crystal

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- Number: US 2021/0277500 A1
- Document ID: US20210277500A1
- Status: Published application
- Kind: A1
- Application number: 17/126,359
- Filed: 2020-12-18
- Published: 2021-09-09
- Earliest claimed: 2020-02-04
- Assignees: Northwestern Polytechnical University
- Applicants: Northwestern Polytechnical University
- Inventors: Wenchao YANG; Jiarun QIN; Pengfei QU; Lin LIU; Jun ZHANG; Haijun SU; Taiwen HUANG; Min GUO; Yueling GUO
- Web page: https://patentgrep.com/patent/US20210277500A1

## CPC

- C22C 1/03: using master alloys
- C22C 19/03: based on nickel
- C22C 30/00: Alloys containing less than 50% by weight of each constituent
- C30B 11/14: characterised by the seed, e.g. its crystallographic orientation
- C30B 15/10: Crucibles or containers for supporting the melt
- C30B 15/16: by irradiation or electric discharge
- C30B 15/24: using mechanical means, e.g. shaping guides (shaping dies for edge-defined film-fed crystal growth C30B15/34)
- C30B 15/36: characterised by the seed, e.g. its crystallographic orientation
- C30B 29/52: Alloys
- C22C: ALLOYS (treatment of alloys C21D, C22F)
- C30B: SINGLE-CRYSTAL GROWTH (by using ultra-high pressure, e.g. for the formation of diamonds, B01J3/06); UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL (zone-refining of metals or alloys C22B); PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE (casting of metals, casting of other substances by the same processes or devices B22D; working of plastics B29; modifying the physical structure of metals or alloys C21D, C22F); SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE (for producing semiconductor devices or parts thereof H10); APPARATUS THEREFOR

## Abstract

In the method for preparing single crystal superalloy test bars by using a Ni—W heterogeneous seed crystal, on the premise of ensuring that the single crystal superalloy has the required orientation, by reusing the seed crystal, it is achieved that the trouble caused by the need of preparing a new seed crystal when a single crystal superalloy is produced by the seed crystal method every time is avoided, and the production cost is significantly reduced. In the present disclosure, the formation of the stray grains in mushy zone could be avoided by using a Ni—W heterogeneous seed crystal without mushy zone and a built-in corundum tube.

## Claims

### Claim 1

A method for preparing single crystal superalloys by using a Ni—W heterogeneous seed crystal, comprising:
step 1, preparing a shell mould;
step 2, preparing a seed crystal for preparing Ni—W heterogeneous single crystal test bars:
preparing a single crystal test bar by a grain selection method;
step 3, preparing a first Ni—W heterogeneous single crystal test bar with a [001] orientation which deviates from the axial direction by 0-12°:
preparing a Ni—W heterogeneous single test bar with a [001] orientation which deviates from the axial direction by 0-12° by using the seed crystal obtained in step 2;
step 4, preparing a first single crystal superalloy test bar:
cutting the obtained first Ni—W heterogeneous single crystal test bar to obtain a Ni—W heterogeneous seed crystal that can be put into the shell mould;
preparing a single crystal superalloy test bar by using the cut Ni—W heterogeneous seed crystal, specifically comprising:
putting the obtained Ni—W heterogeneous seed crystal into the corundum tube in the shell mould; placing the shell mould filled with the Ni—W heterogeneous seed crystal in a directional solidification furnace; putting a purchased superalloy master alloy block into an electromagnetic melting crucible at the upper part of the furnace; heating the directional solidification furnace to a temperature of 1550° C. at a rate of 10° C./min, so as to melt the upper surface of the Ni—W heterogeneous seed crystal near the heater of the directional solidification furnace;
increasing the power of the electromagnetic melting crucible to 7.5 kW, so as to completely melt the superalloy master alloy block in the crucible to obtain a superalloy liquid; casting the superalloy liquid into the shell mould, and full filling the shell mould with the superalloy liquid;
generating a mushy zone with a length of 2-3 mm on the upper part of the Ni—W heterogeneous seed crystal by the cast superalloy liquid and holding for 10 min-30 min, wherein the mushy zone is a solid-liquid two-phase region generated at the joint of the superalloy liquid and the Ni—W heterogeneous seed crystal;
after the holding is completed, subjecting the obtained system to a crystal pulling by pulling down at a rate of 40 μm/s-100 μm/s; after the crystal pulling is completed, taking out the product after the heating furnace is cooled to 300° C., to obtain a first single crystal superalloy test bar with a [001] orientation which deviates from the axial direction by 0-12°;
step 5, recovering the seed crystal for reuse:
recovering the Ni—W heterogeneous seed crystal for reuse from the obtained first single crystal superalloy test bar with a [001] orientation which deviates from the axial direction by 0-12°, specifically comprising:
removing the shell mould on the obtained first single crystal superalloy test bar with a [001] orientation which deviates from the axial direction by 0-12°;
cutting the Ni—W heterogeneous seed crystal from the first single crystal superalloy test bar with a [001] orientation which deviates from the axial direction by 0-12° after the shell mould is removed, and recovering it for reuse; and
step 6, preparing other single crystal superalloy test bars:
preparing other single crystal superalloy test bars by using the obtained recovered seed crystal, wherein the other single crystal superalloy test bars have a [001] orientation which deviates from the axial direction by 0-12°, and the specific process comprises:
putting the recovered seed crystal into the corundum tube in the shell mould; placing the shell mould in a directional solidification furnace, and repeating step 4 to obtain a second superalloy test bar;
repeating step 5 to re-obtain the recovered seed crystal; repeating the process of preparing the second superalloy test bar to obtain a third superalloy test bar;
repeating the processes of recovering seed crystal and preparing superalloy test bar until the required number of superalloy test bars are obtained.

### Claim 2 (depends on 1)

The method as claimed in claim 1, wherein the superalloy master alloy block comprises a DD3 superalloy master alloy block, wherein the DD3 superalloy is the first generation superalloy developed by Beijing Institute of Aeronautical Materials.

### Claim 3 (depends on 1)

The method as claimed in claim 1, wherein the shell mould comprises a casting segment and a seed crystal segment with a corundum tube; the seed crystal segment has a length equal to that of the corundum tube, and before preparing a seed crystal, the corundum tube is put into the seed crystal segment; the corundum tube has an inner diameter of 6.98-11.98 mm and a length of 40 mm.

### Claim 4 (depends on 1)

The method as claimed in claim 1, wherein the process for preparing a seed crystal for preparing the Ni—W heterogeneous single crystal test bar comprises:
directionally cutting a single crystal cylinder with a [001] orientation which deviates from the axial direction by 0-12° from the single crystal test bar and acting as a seed crystal, wherein the directionally cut seed crystal has a [001] orientation which deviates from the axial direction by 0-12°.

### Claim 5 (depends on 4)

The method as claimed in claim 4, wherein the Ni—W heterogeneous seed crystal has a diameter of 6.96-11.94 mm, a length of 35 mm and a gap of 0.02-0.06 mm with the corundum tube.

### Claim 6 (depends on 1)

The method as claimed in claim 1, wherein the specific process for preparing a first Ni—W heterogeneous single test bar with a [001] orientation which deviates from the axial direction by 0-12° comprises:
taking another corundum tube as a container for preparing Ni—W heterogeneous single crystal test bars, wherein the corundum tube has an inner diameter of 6.97-11.98 mm and a length of 115 mm;
using a Ni—W alloy as the master alloy, putting the obtained seed crystal and the Ni—W master alloy into the corundum tube in the order of the seed crystal at the bottom and the Ni—W master alloy on the top; installing the corundum tube filled with the seed crystal and the master alloy on the bottom platform of a LMC directional solidification furnace; and
heating the directional solidification furnace to 1550° C. at a rate of 10° C./min and holding for 40-50 min, so as to melt the master alloy in the corundum tube and form a mushy zone with a length of 2-3 mm on the seed crystal; after the holding is completed, subjecting the obtained system to a crystal pulling by pulling down at a rate of 10 μm/s-100 μm/s; after the crystal pulling is completed, taking out the corundum tube after the directional solidification furnace is cooled to 100° C., to obtain the first Ni—W heterogeneous single crystal test bar with a [001] orientation which deviates from the axial direction by 0-12°, wherein
the first Ni—W heterogeneous single crystal test bar has a diameter of 6.96-11.94 mm, a length of 35 mm, and a gap of 0.02-0.06 mm with the corundum tube.

### Claim 7 (depends on 1)

The method as claimed in claim 1, wherein the Ni—W heterogeneous seed crystal which is cut from the obtained first single crystal supperalloy test bar with a [001] orientation which deviates from the axial direction by 0-12° has a length equal to that of the raw Ni—W heterogeneous seed crystal and a diameter of 6.94-11.90 mm, so as to ensure the gap between the recovered seed crystal and the inner wall of the corundum tube fall within a range of 0.04-0.15 mm.