JPS6217100A - Production of beryl single crystal - Google Patents

Abstract

PURPOSE:To control the generation of a coexistent mineral, to increase the yield of the titled beryl single crystal and to improve the quality by controlling the temp. of the surface of a liq. flux to a specified temp. in the method for growing a bery single crystal by a temp. difference method or an annealing method. CONSTITUTION:One or more kinds selected from V2O5, lithium molybdate, sodium molybdate, potassium molybdate, MoO3 and Li2O is used as the flux, BeO, Al2O3 and SiO2 as the beryl components and Cr2O3 as the colorant are dissolved in the flux and a beryl single crystal is grown by a temp. difference method or an annealing method. In this method, the temp. of the liq. flux surface is controlled in the range -6-2 deg.C with respect to the temp. of the beryl growing part. In the conventional molten salt method, the temp. of the liq. flux surface has been regulated >=10 deg.C lower than the temp. of the beryl growing part. Consequently, the output of beryl is decreased due to the rapid cooling of the liq. flux surface and the transparency is deteriorated. The problems can be solved by this method, the yield of the beryl single crystal is increased and the quality is also improved.

Description

DETAILED DESCRIPTION OF THE INVENTION [Industrial Application Minute Hand] The present invention relates to a method for supplementing beryl single crystals by a molten salt (flux) method.

[Summary of the invention]

The present invention improves the quality of the obtained crystals by controlling the beryl single crystals using a temperature difference method or slow cooling method, suppressing the generation of coexisting minerals.

(Conventional technology) - In the conventional molten salt method, the temperature of the flux liquid surface is
(Problems and objectives to be solved by the invention) However, in the above-mentioned prior art, the flux liquid surface cools down rapidly. This has the problem of having a serious impact on quality, such as reducing the amount of beryl produced, and being burrowed in as inclusions during growth, reducing transparency.

The present invention is intended to solve the above-mentioned problems, and its purpose is to increase the yield of beryl single crystals and provide a method for producing t-beryl single crystals with excellent quality.

(Ninth Means for Solving the Problems) The beryl single crystal production method of the present invention uses flux [Examples] The method of the present invention will be described below based on Examples.

[Example-1] (1) # agent (flux) '/20s ToLi0Hfj20: 1(7)'
Use jLf &TeIK#.

(2) Melting method Φ Using a PT crucible and a crucible furnace, the above flux 11
Melts at 000℃.

■ Control the temperature of the beryl growing part so that it is 5°C lower than the temperature of the bottom of the crucible, and further check the flux level and the beryl growing part [part t - 7 as shown in Table 1]. : y to 3 types of temperature difference! if
control

(2) A mixed sintered body of At, O327t and Be010f is introduced and melted.

■ Three days later, At! The dissolution of 03 and Boo is checked using an emission spectrometer II.

It is confirmed by analysis that each component has dissolved at least 80% of Kamewayu'si.

■ C,,r! as a doping agent! The os sintered body was heated to 1.1f (
At weight ratio: 4.1 h of At, 03) and dissolve.

■　810. Add 55p of (crystal) and dissolve.

After two days, use an emission spectrometer to check whether each raw material is saturated or not. It is confirmed by analysis that each of the 66 components has dissolved at least 80eI6, which is the saturated dissolution amount.

(3) Cultivating Beryl ■ Add beryl crystal pieces for t-2 days to confirm improvement.

Check the growth status and presence or absence of coexisting minerals.

■ Insert beryl seed crystal pieces for breeding.

■ Raise the temperature of the flux by 15°C and hold for 24 hours to etch the surface of the seed crystal.

■ Slowly cool to the original temperature at a slow cooling rate of 4°C/d a, y.

■ After the slow cooling is completed, a mixed sintered body of At, am and BaO (a mixed sintered body in which the ratio of Azlo3, Bc, and O is 3=1 by weight), a sintered body of Cr103, crystal t
-Additionally every 7 days and grow for 60 days. (The amount of raw materials and raw materials to be added is determined each time by analysis using an emission spectrometer.) 17j. As a comparative example, the temperature difference between the flux level and the beryl growing area is outside the above range. Prepare two odes and train them to be the same.

(4) Quality check: Check the amount of seed crystal growth and check whether the seed surface contains coexisting minerals.

(result) The amount of crystal growth, ' and quality evaluation are shown in Table 1 below.

In Table 1, the degree to which the temperature of the flux liquid surface is changed relative to the temperature of the beryl growing area is expressed as Δ.

As is clear from Table 1, within the scope of the claims of the present invention, extremely high quality single crystals containing no coexisting minerals can be obtained.

On the other hand, in Comparative Examples 1 and 2, which are outside the above-mentioned range, inclusion of coexisting minerals is observed in 1, and very little beryl grows in 2, so they are not practical.

[Example-2] (1) Solvent (flux) Same as Example-1.

(2) Dissolution method Same as Example-1.

(3) Cultivating Beryl Same as Example-1■ to ■.

■ Slowly cool to 100°C at a slow cooling rate of 4°C/d ay.

As a comparative example, two types were prepared in which the temperature difference between the flux level and the beryl growing area was outside the above-mentioned range, and the beryl was grown in the same manner.

(4) Quality check Same as Example-1.

(Results) The crystal growth and quality evaluation are as follows! It is shown in Table gg2. In addition, in Table 2, the number of times the temperature of the flux liquid surface is changed relative to m degrees of the beryl growing area is expressed as ΔT.

As is clear from Table M2, within the scope of the claims of the present invention, extremely high quality beryl single crystals containing no coexisting minerals can be obtained.

On the other hand, in Comparative Examples 1 and 2, which are outside the above-mentioned range, inclusion of coexisting minerals is observed in 1, and very little beryl grows in 2, so they are not practical.

[Example 1-3] (1) Solvent (7 lux) L12MOO4 and Mo03i are used in a ratio of 1 to 1:1.

(2) Melting method ■ Melt the upper 6 flux at a melting temperature of 900°C. The equipment and jig are the same as in Example-1.

■ The temperature of the flux liquid surface and the temperature of the beryl growing part are
The temperature is controlled to three different temperature differences as shown in the table.

(2) A mixed sintered body of At, 0315f and Be08f is charged and melted.

(3) After 3 days, check the dissolved amounts of *t2 o3 and BeO using an emission spectrometer e+.

Analyze and confirm that each component has dissolved at least 80% of the cystocyst.

(2) Add α7 to the Cr2O3 sintered body as a doping agent and dissolve it.

■　810! (Crystal) Add t-35f and dissolve.

■ After 2 days, are each raw material saturated?
: Check using an emission spectrometer.

It is confirmed by analysis that each component is dissolved in a saturated amount of 80 or more.

(3) Same as Beryl Growth Example-1 (4) Same as Quality Check Example-1 (Results) The amount of crystal growth and quality evaluation are shown in Table 3 below. In Table 3, the number of times the temperature of the flux liquid surface is changed relative to the temperature of the beryl growing area is expressed as ΔT.

As is clear from Tables 3 and 5, very high quality beryl single crystals containing no coexisting minerals can be obtained within the scope of the claims of the present invention.

On the other hand, in Comparative Examples 1 and 2, which are outside the above-mentioned range, in 1, coexistence mineral envelopment M is observed, and in 2, beryl grows very little, making it impractical.

〔Effect of the invention〕

As mentioned above, the production of the beryl single crystal of the present invention is advantageous in that the generation of coexisting minerals can be suppressed, thereby increasing the yield and improving the quality.

The present invention has great effects as a method for synthesizing artificial beryl single crystals.

that's all

Claims (1)

[Claims] One or more selected from vanadium pentoxide, lithium molybdate, sodium molybdate, potassium molybdate, molybdenum trioxide, and lithium oxide are used as a solvent (flux), and the oxidized beryl component is used as a solvent (flux). Beryllium (BeO), aluminum oxide (A
1_2O_3), silicon dioxide (SiO_2), and chromium oxide (Cr_2O_3) as a coloring agent to grow a beryl single crystal by a temperature difference method or slow cooling method, in which the temperature of the flux liquid surface is adjusted to the temperature of the beryl growth zone. A method for producing a beryl single crystal, characterized in that the temperature is controlled within a range of -6°C to 2°C.