CN1115428C - Method for growing monocrystal of yttrium boride - Google Patents
Method for growing monocrystal of yttrium boride Download PDFInfo
- Publication number
- CN1115428C CN1115428C CN 00130361 CN00130361A CN1115428C CN 1115428 C CN1115428 C CN 1115428C CN 00130361 CN00130361 CN 00130361 CN 00130361 A CN00130361 A CN 00130361A CN 1115428 C CN1115428 C CN 1115428C
- Authority
- CN
- China
- Prior art keywords
- growing
- molten salt
- present
- single crystal
- speed
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Fee Related
Links
Abstract
The present invention relates to a monocrystal molten salt seed crystal pulling growth method. The present invention has the steps of raw material synthesizing, stock melting, seed crystal delivering and growing. A metal Y is used as a fluxing agent, directional seed crystals are adopted, the seed crystals grow under the condition of temperature drop at a speed of 1 to 10 DEG C /h, and 1 to 25 revolutions/minute of the rotary speed and 1 to 20 mm/h of the pulling speed are matched with the growth speed of the seed crystals. The method of the present invention can be used for stably growing YB2 monocrystals. Compared with the YB2 monocrystals grown by a molten salt slow cooling method, the YB2 monocrystals grown by the method of the present invention are crystals with large size and good completeness. Compared with a zone melting method, the present invention has the advantages of simple technological equipment and convenient operation because the whole technical process from the raw material synthesizing to the growing can be accomplished in one time.
Description
The invention relates to a single crystal growth method, in particular to a fused salt seed crystal pulling method growth method of single crystals.
YB2The single crystal belongs to a hexagonal crystal system, the space group is P6/mmm, the lattice constant a is 3.299 Å, and c is 3.826 Å2The melting point is up to 2100 ℃, at which temperatureYB2The melt has high chemical activity, and most of materials are almost similar to YB2The melt undergoes chemical reactions, so that YB growth has not been found for a long time2Suitable crucible materials for single crystals are used. Currently YB2The single crystal growth is generally carried out by the float zone method (document 1, Robert. W. Johnson, Journal of applied Physics, 34(2) (1963) p352) for growing YB2Single crystals, first of all YB is synthesized in an arc melting apparatus2Polycrystalline and then made into YB in a water-cooled copper crucible2Polycrystalline rods, finally growing in a zone melting device. The whole process from raw material synthesis to growth is complex.
We are at YB2The research work of single crystal growth finds that: BN to YB2The melt does not cause pollution and is suitable for YB2A crucible material for single crystal growth. Using metal Y as fluxing agent, in BN crucible, utilizing induction heating to grow YB with 2-5mm of linearity and good quality by slow cooling method2And (3) single crystal. However, the crystal growth by this method is through spontaneous nucleation, and it is very difficult to control the spontaneous nucleation of a few crystal grains, so that it is not easy to obtain YB of large size2And (3) single crystal.
The invention aims to provide a method for simply and conveniently growing large-size YB2Method for growing YB (Yb-Yb) by using molten salt seed crystal pulling method2And (3) single crystal. Due to YB2Has the characteristics of metal, lower resistivity and high thermal conductivity, and can grow at a faster cooling rate.
The purpose of the invention is realized as follows:
(1) using metal Y as fluxing agent, mixing YB in a certain proportion4Powder and excess metal Y (so that YB is2The molar ratio of Y to Y is controlled within the range of 3: 2-9: 1) is placed in a BN crucible, a tungsten cylinder or a tantalum cylinder sleeved outside the crucible is used as a heating body, MgO or ZrO refractory heat-insulating material is filled between the heating body and a quartz glass cup, the heating body and the quartz glass cup are vacuumized, then high-purity argon is filled as protective gas, the materials are heated to the melting point (1520 ℃) of metal Y by medium-frequency induction heating, and YB4And (2) processThe amount of metal Y is reacted according to the following reaction: generating YB2。
(2) Raising the temperature to 2000-2100 ℃ according to different proportions of solute and fluxing agent to ensure that YB is heated4All converted into YB2And YB2And the excess metal Y is in a molten state. Keeping the temperature for 3-5h to mix evenly.
(3) And cooling to a temperature slightly higher than the saturation point, after the temperature is balanced, adopting directional seed crystals, discharging the seed crystals, and keeping the temperature for 1-2 hours.
(4) Cooling to saturation point, after temperature is balanced, slowly cooling at a cooling speed of 1-10 deg.C/h, starting crystal growth, and controlling crystal rotation speed to 1-25 rpm, wherein crystal pulling speed is 1-20 mm/h.
(5) When the crystal grows to the required size, the crystal is lifted out of the liquid surface and cooled to the room temperature at the cooling rate of 50-60 ℃/h, and then enough YB can be obtained2And (4) crystals.
YB grown by the invention2And (3) measuring the crystal structure of the single crystal, wherein each structural parameter is basically consistent with data reported by data. YB (Yb)2The half-peak width of the X-ray rocking curve of the single crystal is 7-10arcsec, which shows that the crystal quality of the crystal is good.
The invention uses a fused salt seed crystal pulling method to grow YB2Single crystals, in contrast to the molten salt slow cooling method, canTo obtain YB of large size2Single crystal, and the whole technological process of raw material synthesis and growth can be completed at one time; compared with the zone melting method, the whole process from raw material synthesis to growth is simple and easy to operate.
Example 1
138.02g of YB with a purity of 99.5% will be accurately weighed4113.50g of metal Y having a purity of 99.9% (corresponding to YB)2And Y molar ratio of 9: 1) is placed in a BN crucible with the diameter of 40mm multiplied by 70mm, a tungsten cylinder or a tantalum cylinder sleeved outside the crucible is used as a heating body, MgO or ZrO particle fireproof heat-insulating material is filled between the heating body and a quartz glass cup, the heating body and the quartz glass cup are vacuumized, then high-purity Ar gas is filled as protective gas, and the materials are heated by medium-frequency induction to obtain the materialHeating to 1520 deg.C, YB4Reacting with excess metal Y to form YB230 minutes later, the temperature is raised to 2100 ℃ to let YB stand4All converted into YB2And YB2And metal Y is in a molten state. Keeping the temperature for 3-5h to mix evenly. Then quickly cooling to a temperature slightly higher than the saturation point, and after the temperature is balanced, adopting [0001]]And (4) adding seed crystals, keeping the temperature for 1h, and rapidly cooling to the temperature of the saturation point. After temperature balance, slowly cooling at a cooling speed of 4 ℃/h, starting crystal growth, and controlling the crystal rotation speed to be 22-25 rpm, wherein the crystal pulling speed is 20 mm/h. When the crystal grows to the required size, the crystal is taken out of the liquid level and cooled to the room temperature at the cooling rate of about 50 ℃/h, and then the YB with the phi of 20mm multiplied by 60mm can be obtained2And (3) single crystal.
Example 2
108.65g of YB with a purity of 99.5% will be accurately weighed4135.75g of metal Y having a purity of 99.9% (corresponding to YB)2And Y in a molar ratio of 7: 3) were placed in a BN crucible having a diameter of 40mm by 70mm, as in example 1. Seed crystal orientation of [0100]]After the direction and the temperature are balanced, the temperature is slowly reduced at the speed of 10 ℃/h, the crystal starts to grow, and the rotating speed of the crystal is controlled to be 8-10 DEG CRpm and a crystal pulling rate of 10 mm/h. When the crystal grows to the required size, the crystal is taken out of the liquid level and cooled to the room temperature at the cooling rate of about 50 ℃/h, and then the YB with the phi of 20mm multiplied by 40mm can be obtained2And (3) single crystal.
Example 3
93.69g of YB with a purity of 99.5% is accurately weighed4147.07g of metal Y having a purity of 99.9% (corresponding to YB)2And Y in a molar ratio of 3: 2) were placed in a BN crucible having a diameter of 40mm by 70mm, as in example 1. After 30 minutes, the temperature is raised to 2050 ℃ to let YB stand4All converted into YB2And YB2And metal Y is in a molten state. Keeping the temperature for 3-5h to mix evenly. Then quickly cooling to a temperature slightly higher than the saturation point by 5-10 ℃, and after the temperature is balanced, adopting [2000]]Directional seed crystals, seed crystals are placed, the temperature is kept for 1-2h, and the temperature is rapidly reduced to the temperature of a saturation point. After temperature balance, slowly cooling at a cooling speed of 1 ℃/h, starting crystal growth, controlling the rotation speed of the crystal to be 1-3 rpm, and pulling the crystalThe speed was 1 mm/h. When the crystal grows to the required size, the crystal is taken out of the liquid level and cooled to the room temperature at the cooling rate of about 50 ℃/h, and then the YB with the phi of 20mm multiplied by 20mm can be obtained2And (3) single crystal.
Claims (6)
1. A method for growing yttrium boride single crystal by molten salt pulling technology comprises the steps of melting prepared raw materials and fluxing agent in a crucible, seeding, and slowly cooling to grow, and is characterized in that: yttrium metal is used as fluxing agent and solute YB of raw material2The mol ratio of the fluxing agent to the flux Y is 3: 2-9: 1.
2. The molten salt pulling method for growing a yttrium boride single crystal according to claim 1, characterized in that: and (3) adopting oriented seed crystals, wherein the direction is selected from [0001], [0100], [2000] or [0202 ].
3. The molten salt pulling method for growing a yttrium boride single crystal according to claim 1, characterized in that: the cooling rate is 1-10 ℃/h.
4. The molten salt pulling method for growing a yttrium boride single crystal according to claim 1, characterized in that: the rotation speed of the seed crystal is 1-25 r/min.
5. The molten salt pulling method for growing a yttrium boride single crystal according to claim 1, characterized in that: the seed crystal pulling speed is 1-20 mm/h.
6. The molten salt pulling method for growing a yttrium boride single crystal according to claim 1, characterized in that: wherein the crucible is made of BN.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 00130361 CN1115428C (en) | 2000-11-02 | 2000-11-02 | Method for growing monocrystal of yttrium boride |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 00130361 CN1115428C (en) | 2000-11-02 | 2000-11-02 | Method for growing monocrystal of yttrium boride |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1353215A CN1353215A (en) | 2002-06-12 |
| CN1115428C true CN1115428C (en) | 2003-07-23 |
Family
ID=4594129
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 00130361 Expired - Fee Related CN1115428C (en) | 2000-11-02 | 2000-11-02 | Method for growing monocrystal of yttrium boride |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1115428C (en) |
-
2000
- 2000-11-02 CN CN 00130361 patent/CN1115428C/en not_active Expired - Fee Related
Also Published As
| Publication number | Publication date |
|---|---|
| CN1353215A (en) | 2002-06-12 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| JP2003277197A (en) | CdTe SINGLE CRYSTAL, CdTe POLYCRYSTAL AND METHOD FOR PRODUCING THE SINGLE CRYSTAL | |
| JP2002293693A (en) | Terbium-aluminum-garnet single crystal and method of manufacturing for the same | |
| US4303465A (en) | Method of growing monocrystals of corundum from a melt | |
| Linares | Growth of Single‐Crystal Garnets by a Modified Pulling Technique | |
| JP4788524B2 (en) | Group 13 metal nitride crystal production methods and solutions and melts used in these production methods | |
| Péter et al. | Synthesis and crystallization of lithium-yttrium orthoborate Li6Y (BO3) 3 phase | |
| Oliver et al. | Growth of single crystal YB66 from the melt | |
| EP1132505B1 (en) | Method for producing single-crystal silicon carbide | |
| CN1115428C (en) | Method for growing monocrystal of yttrium boride | |
| JP4609207B2 (en) | Periodic table group 13 metal nitride crystal manufacturing method and semiconductor device manufacturing method using the same | |
| TWI287592B (en) | InP single crystal wafer and InP single crystal manufacturing method | |
| JP2005112718A5 (en) | ||
| JP5252002B2 (en) | Group 13 metal nitride crystal manufacturing method and semiconductor device manufacturing method | |
| CN113788480A (en) | Preparation method of high-purity silicon carbide and corresponding high-purity silicon carbide | |
| JP2000344595A (en) | Method and apparatus for producing oxide single crystal | |
| WO2001048277A1 (en) | Method and apparatus for producing single crystal of silicon carbide | |
| JP2010105903A (en) | Method for producing group 13 metal nitride crystal and method for producing semiconductor device | |
| Otani et al. | Preparation of LaB6 single crystals by the floating zone method | |
| JP4778188B2 (en) | Method for producing compound semiconductor single crystal | |
| KR20090042202A (en) | Single-crystal sic and process for producing the same | |
| JP2004203721A (en) | Apparatus and method for growing single crystal | |
| US5336362A (en) | Method for preparing yttrium 66 boride crystal for soft x-ray monochromator | |
| CN116607211B (en) | Charging method for solid phase synthesis of silicon carbide and synthesis method | |
| JP2997761B2 (en) | Method for producing rhenium diboride single crystal | |
| JP2580523B2 (en) | Growth method of titanium diboride single crystal |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C06 | Publication | ||
| PB01 | Publication | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| C19 | Lapse of patent right due to non-payment of the annual fee | ||
| CF01 | Termination of patent right due to non-payment of annual fee |