JP2015089923A - Method of producing inorganic compound - Google Patents

Abstract

PROBLEM TO BE SOLVED: To obtain an inorganic compound (inorganic phosphor) strong in emission intensity.SOLUTION: An inorganic compound is obtained by decomposing the high-energy material in the closed vessel in a state where an inorganic composition containing a compound semiconductor and a doping agent and a high-energy material prepared by mixing a carbon-free hydrazine nitrate (HN) with a water-saturated hydrazine (HH) are sealed in a closed vessel. The method of producing an inorganic compound by using the high-energy material prepared by mixing hydrazine nitrate and water-saturated hydrazine eliminates the possibility of mixing of carbon residue inhibiting light emission, resulting in an inorganic compound strong in emission intensity.

Description

  The present invention relates to a manufacturing method for manufacturing an inorganic compound used for manufacturing an inorganic EL element.

  In recent years, EL elements (electroluminescence elements) have attracted attention as light-weight and thin surface-emitting elements. Since EL elements have such features as high definition, high contrast, and high response speed, they are used in backlights for liquid crystal displays, various interior lighting devices, in-vehicle display devices, and the like.

  The EL elements are roughly classified into organic EL elements and inorganic EL elements. Inorganic EL elements include a dispersion-type inorganic EL element that uses a phosphor layer in which inorganic phosphor particles are dispersed in a binder, and a thin-film inorganic EL element that uses a thin film made of an inorganic phosphor. In such an inorganic EL element, for example, a zinc sulfide-based (ZnS-based) inorganic compound is used as the inorganic phosphor.

  As a method for producing an inorganic compound (inorganic phosphor), there is a method of doping an inorganic composition with an iridium element or the like. For example, Patent Document 1 discloses that an inorganic composition containing a compound semiconductor (ZnS or the like) and an iridium element is placed in a sealed container together with explosives TNT (trinitrotoluene) in the sealed container. A method of producing an inorganic composite (inorganic compound) by heating and blasting (doping treatment) has been proposed.

  Patent Document 2 also proposes a method for producing a phosphor by thermally decomposing an exothermic decomposable compound (such as TNT) in a sealed container.

JP-T 2009-511645 JP 2012-072376 A

  By the way, when a heat treatment (doping treatment) is performed using TNT as in Patent Document 1 described above, carbon, which is a reaction residue of TNT, is mixed in the inorganic compound, resulting in poor luminous efficiency. That is, light absorption occurs due to black contamination by carbon, and the emission intensity decreases. In addition, when carbon is mixed in an inorganic compound, there remains an influence such as film formation processing (evaporation or the like) at the time of manufacturing an EL element becoming unstable.

  In Patent Document 2, as a method for removing carbon (reaction residue) adhering to the phosphor, a method is proposed in which the phosphor is fired in an atmosphere in which oxygen is mixed to oxidize / disappear the carbon. However, in such a method, the target semiconductor compound such as ZnS is also oxidized, so that the light emission efficiency is impaired.

  The present invention has been made in view of such circumstances, and an object thereof is to provide a method for producing an inorganic compound (inorganic phosphor) having high emission intensity.

First, since carbon is contained in TNT, a carbon residue is generated when the above heat treatment (doping treatment) is performed using TNT. Therefore, the inventor of the present invention pays attention to hydrazine nitrate (HN) as a high-energy substance not containing carbon, and when the inorganic composition is heated (doping treatment) using the hydrazine nitrate, It has been found that an inorganic phosphor (inorganic compound) having a higher emission intensity than when TNT is used can be produced. However, hydrazine nitrate ((NH ₂ ) ₂ HNO ₃ ) generates oxygen by the following reaction during decomposition.

_{H 5 N 3 O 3 ⇒ 2.5H} 2 O + 1.5N 2 + 0.5O 2
For this reason, when hydrazine nitrate is used as a high-energy substance, the atmosphere during the reaction (the atmosphere in the sealed container) becomes an oxygen atmosphere, and a reaction byproduct (for example, barium sulfate) is generated by the reaction from the oxygen. End up. When such a reaction by-product is contained in the inorganic compound, the film formation process (evaporation or the like) at the time of manufacturing the EL element becomes unstable, and the productivity of the inorganic EL element is lowered.

  Therefore, the inventors of the present invention have studied about making the inside of a sealed container in a reducing atmosphere at the time of heat treatment even when hydrazine nitrate is used. As a result, hydrazine nitrate is mixed with saturated hydrazine (HH), and the hydrazine nitrate is mixed with hydrazine nitrate. By selecting a mixing ratio with saturated hydrazine, it was newly found out that the inside of a sealed container at the time of heat treatment can be made a reducing atmosphere, and the present invention was invented.

  That is, the present invention provides a method for producing an inorganic compound used for producing an inorganic EL device, wherein an inorganic composition containing a compound semiconductor and a high-energy substance obtained by mixing hydrazine nitrate and saturated hydrazine are contained in a sealed container. A technical feature is that the energetic substance in the sealed container is thermally decomposed by heating in the sealed state.

  According to the present invention, an inorganic compound is produced by applying high temperature and high pressure to an inorganic composition (containing a compound semiconductor) using a high-energy substance obtained by mixing hydrazine nitrate not containing carbon and saturated hydrazine. Therefore, the inorganic compound (inorganic phosphor) does not contain a carbon residue that inhibits light emission. Thereby, the emission intensity of the inorganic compound can be increased.

  In addition, by selecting the mixing ratio of hydrazine nitrate and saturated hydrazine constituting the high energy substance, the atmosphere in the sealed container when the high energy substance decomposes in the sealed container can be reduced. Therefore, it is possible to prevent the by-product (for example, barium sulfate) from being included in the inorganic compound used for manufacturing the inorganic EL element. Thereby, the film-forming process (evaporation etc.) at the time of EL element production can be performed stably.

  Furthermore, hydrazine nitrate and saturated hydrazine are not explosives as defined in Chapter 1 and Article 2 of the Explosives Control Law, so they must be handled in accordance with the Explosives Control Law during transportation, storage, and manufacturing. There is no, and the handleability is good.

  Note that “explosives” is defined as “explosives”, “explosives”, and “pyrotechnics” in Chapter 1 of Article 1 of the Explosives Control Law. “Explosives” means “explosives for use in propulsion explosions and specified by the Ordinance of the Ministry of Economy, Trade and Industry”. “Explosives” means “explosives for use in destructive explosions, It is defined as what is specified by a ministerial ordinance. In this way, in Chapter 1 of Article 1 of the Explosives Control Law, things that are subject to propulsion explosions and destructive explosions are defined as “explosives”, and hydrazine nitrate and saturated hydrazine are not used for such purposes. So it's not "explosives".

  According to the present invention, an inorganic compound having high emission intensity can be produced.

It is a figure which shows typically an example of the manufacturing apparatus which implement | achieves the manufacturing method of the inorganic compound of this invention. It is a graph which shows the relationship between the weight ratio of hydrazine nitrate (HN) and saturated hydrazine (HH), and oxygen balance. It is a figure which shows the result of having measured the PL intensity | strength of the inorganic compound produced by the Example and comparative example of this invention. It is a figure which shows the result of having measured the X-ray-diffraction peak of the inorganic compound produced by the Example and comparative example of this invention. It is a figure which shows the result of having measured the X-ray-diffraction peak of the inorganic compound produced by the Example and comparative example of this invention.

  Hereinafter, embodiments of the present invention will be described with reference to the drawings.

[manufacturing device]
First, the manufacturing apparatus which implement | achieves the manufacturing method of the inorganic compound of this invention is demonstrated with reference to FIG.

  The manufacturing apparatus of this example includes an airtight container 1, a heating furnace 2, a gas burner 3, and the like.

  The sealed container 1 is a stainless steel container having an internal volume of 100 mL, and includes a container body 11 and a lid body 12. The container body 11 is a cylindrical container having an outer diameter of φ100 mm and a height of 170 mm (an inner diameter of φ40 mm and an inner height of 120 mm), and only the upper part is opened. The lid 12 is a cylindrical body having an outer diameter of φ100 mm (same as the container body 1) and a height of 40 mm. The inside of the sealed container 1 can be sealed by fastening the lid 12 to the container body 1 using a hexagon socket bolt 13.

  The heating furnace 2 is composed of a heat-resistant brick or the like, and can accommodate the sealed container 1 therein. A gas burner 3 is disposed below the heating furnace 2, and the sealed container 1 accommodated in the heating furnace 2 can be heated by the gas burner 3.

  And when manufacturing an inorganic compound (inorganic fluorescent substance) using the manufacturing apparatus of this example, (i) The raw material M which mixed the compound semiconductor (inorganic composition), the doping agent, etc. in the inside of the container main body 11 is thrown. A high energy substance (liquid) E in which hydrazine nitrate and saturated hydrazine are mixed is put on the raw material M. (Ii) The raw material M and the high energy substance E are sealed in the sealed container 1 by closing the opening of the container body 11 with the lid 12. (Iii) The sealed container 1 in which the raw material M and the high-energy substance E are enclosed is disposed inside the heating furnace 2, and the sealed container 1 is heated by the gas burner 3 in this state.

  When the sealed container 1 is heated in this way, the high-energy substance E in the sealed container 1 is thermally decomposed and high temperature and high pressure are applied to the raw material M (doping treatment). By such treatment, an inorganic compound (inorganic phosphor) used for manufacturing an inorganic EL element can be manufactured.

  And an inorganic EL element is producible by forming into a film on the glass substrate in which transparent electrodes, such as ITO (Indium Tin Oxide), were formed in this way. Examples of the film forming method include EB (ion beam) vapor deposition, sputtering, ion plating, and flash.

  Next, [compound semiconductor], [activator], [sintering aid], and [high energy substance] used in the production of the inorganic compound will be described.

[Compound semiconductor]
Compound semiconductors include zinc sulfide (ZnS), zinc oxide (ZnO), zinc selenide (ZnSe), zinc telluride (ZnTe), cadmium sulfide (Cds), cadmium selenide (CdSe), strontium oxide (SrO), Examples include II-VI group compound semiconductors such as strontium sulfide (SrS), strontium selenide (SeSr), and strontium telluride (SrTe). In the embodiment of the present invention, zinc sulfide (ZnS) is used as the compound semiconductor.

  As compound semiconductors, III-V groups such as gallium nitride (GaN), gallium phosphide (GaP), gallium arsenide (GaAs), indium nitride (InN), indium phosphide (InP), indium arsenide (InAs), etc. A compound semiconductor can be mentioned.

  In addition to these II-VI compound semiconductors and III-V compound semiconductors, group IV compound semiconductors, group I-VI compound semiconductors, group I-VII compound semiconductors, group II-IV compound semiconductors, group II-V A compound semiconductor such as a compound semiconductor or a II-VII group compound semiconductor or a III-VI group compound semiconductor may be used.

[Activator]
The activator becomes a light emission center by doping the compound semiconductor. Examples of the activator include manganese, copper, silver, gold, iridium, yttrium, europium, praseodymium, and terbium. In the examples of the present invention, manganese sulfate (MnSO ₄ ) and iridium chloride (IrCl ₃ ) are used as activators.

[Sintering aid]
The sintering aid is an inorganic compound having a melting point, and when the melt is melted, the above activator is rapidly doped, and the crystal growth is promoted by promoting grain growth of the phosphor base material. . As sintering aids, oxides such as zinc oxide (ZnO) and cadmium oxide (CdO), alkali metal halides such as sodium chloride (NaCl) and lithium chloride (LiCl), magnesium chloride (MgCl ₂ ), fluoride Alkaline earth metal halides such as barium (BaF ₂ ) can be mentioned. In the embodiment of the present invention, zinc oxide (ZnO), barium fluoride (BaF ₂ ), magnesium chloride (MgCl ₂ ), and sodium chloride (NaCl) are used as sintering aids.

[High energy materials]
As described above, when heat treatment (doping treatment) of the inorganic composition is performed using hydrazine nitrate as a high-energy substance, a phosphor having higher emission intensity than that using TNT can be manufactured (described later). See [Example] and [Comparative Example]). However, when only hydrazine nitrate is used as a high-energy substance, the atmosphere during the reaction (the atmosphere in the sealed container) becomes an oxygen atmosphere, so that a reaction by-product (barium sulfate) is generated (the following generation) See mechanism). Therefore, in the present invention, by mixing saturated hydrazine with hydrazine nitrate and selecting the mixing ratio of the hydrazine nitrate and saturated hydrazine, the oxygen balance (OB) of the high energy substance is made negative, and the heat treatment is performed. The inside of the sealed container 1 is made a reducing atmosphere.

-Mechanism of reaction by-product (barium sulfate)-
As described above, since hydrazine nitrate generates oxygen during decomposition, the following reaction occurs from the oxygen, and barium sulfate (BaSO ₄ ) is generated. Since barium sulfate is insoluble in water, it cannot be removed by washing with water.

ZnS + 2O ₂ ⇒ZnSO _{4
^{BaF 2 + SO 4 2- ⇒BaSO 4}} ↓ + 2F -
[Oxygen balance of high energy substances]
Next, the oxygen balance of the high energy material will be described.

First, hydrazine nitrate ((NH ₂ ) ₂ HNO ₃ ) exhibits the reaction [H ₅ N ₃ O ₃ ⇒2.5H ₂ O + 1.5N ₂ + 0.5O ₂ ] as described above during decomposition, and the oxygen balance is + 8.4%.

On the other hand, saturated hydrazine ((NH ₂ ) ₂ H ₂ O) exhibits the following reaction during decomposition, and the oxygen balance is -63.9%.

H ₆ N ₂ O ⇒ 3H ₂ O + N ₂ -1.5O ₂
The oxygen balance (OB) of the compound C _a H _b N _c O _d is generally determined by the following formula.

OB% = [− 1600 / molecular weight] × (2a + (b / 2) −d)
However, a = carbon, b = hydrogen, c = nitrogen, d = oxygen, the molecular weight of the object (HN = 95.06, HH = 50.06)
Here, in the high energy substance (HN / HH) in which hydrazine nitrate and saturated hydrazine are mixed, when the weight ratio of hydrazine nitrate is X wt%, the high energy substance in the case where the hydrazine nitrate is X wt% Oxygen balance (OB)
OB = + 8.4 × (X / 100) + (− 63.9) × {(100−X) / 100)} (1)
It can be expressed as. Thus, the oxygen balance of the high energy substance (HN / HH) is proportional to the weight ratio of hydrazine nitrate (HN weight ratio). When the relationship between the HN weight ratio (% by weight) and the oxygen balance is represented by a graph, a linear graph as shown in FIG. 2 is obtained.

  In the graph of FIG. 2, when the HN weight ratio is 100% by weight (when the high-energy substance is composed only of hydrazine nitrate), the oxygen balance is the above value (+ 8.4%). When the HN weight ratio is 0% by weight (when the high-energy substance is composed only of saturated hydrazine), the oxygen balance is the above value (−63.9%).

  Further, for example, as shown in FIG. 2, the HN weight ratio is 63.5 wt%, and the saturated water hydrazine weight ratio (HH weight ratio) is 36.5 wt% (HN: HH = 63. 5: 36.5, in the case of [Example 1-1] and [Example 2-1] described later), the oxygen balance is -18.0% from the above (1) (OB = + 8.4 ×). 0.635 + (− 63.9) × 0.365 = −18.0%).

  For example, as shown in FIG. 2, when the HN weight ratio is 55.0 wt% and the HH weight ratio is 45.0 wt% (HN: HH = 55.0: 45.0, which will be described later. In the case of [Example 2-2], the oxygen balance is −24.1% from the above (1) (OB = + 8.4 × 0.55 + (− 63.9) × 0.45 = −24). .1%).

  2 and the above equation (1), it can be seen that the oxygen balance of the high energy substance (HN / HH) can be made negative by controlling the HN weight ratio to 88 wt% or less.

  Examples of the present invention will be described together with comparative examples.

[Example 1-1]
<Raw material M>
Zinc sulfide (ZnS) is used as the compound semiconductor. Further, as an activator, manganese sulfate (MnSO ₄ ), iridium chloride (IrCl ₃ ), and as a sintering aid, zinc oxide (ZnO), barium fluoride (BaF ₂ ), magnesium chloride (MgCl ₂ ), sodium chloride ( NaCl). A raw material M was prepared by mixing these ZnS, MnSO ₄ , ZnO, BaF ₂ , MgCl ₂ , IrCl ₃ , and NaCl at a weight percentage shown in Table 1 below.

<High energy materials>
A high energy substance E was prepared by mixing 63.5% by weight of hydrazine nitrate and 36.5% by weight of saturated hydrazine (HN / HH).

<Preparation of inorganic compounds>
The raw material M: 68.0 g and the high energy substance E: 20 g mixed at the above weight ratio (% by weight) are sealed in the sealed container 1 shown in FIG. 1, and the sealed container 1 is placed in the heating furnace 2. In the accommodated state, the hermetic container 1 was heated by the gas burner 3 and a process (doping process) for thermally decomposing the high energy substance E in the hermetic container 1 was performed to produce an inorganic compound (blue phosphor). The heating was continued until the temperature in the sealed container 1 reached about 200 ° C., and the completion of the reaction was confirmed by monitoring the increase in pressure inside the sealed container 1. Next, the sealed container 1 was cooled and degassed, and then the inorganic compound was taken out from the sealed container 1 and washed with water.

  PL (photoluminescence) intensity | strength was measured about the inorganic compound produced by the above process. The PL intensity was measured by irradiating an inorganic compound with light having an excitation wavelength of 325 nm from a He—Cd laser, and using a spectroscope: USB4000 (manufactured by Ocean Optics). The result is shown in FIG. In addition, in FIG. 3, it represents with the relative intensity | strength which made PL intensity | strength of the inorganic compound produced by the following [comparative example 1-2] "1".

  In addition, X-ray diffraction of the above inorganic compound was performed using an X-ray diffractometer: RINT2200 (manufactured by Rigaku Corporation) by an X-ray diffraction method [θ-2θ method, target: Cu, tube voltage: 40 kV, tube current: 30 mA]. The peak (XRD peak) was measured. The X-ray diffraction results are shown in FIG.

[Comparative Example 1-1]
In [Example 1-1] described above, an inorganic compound (blue phosphor) was produced in the same manner as [Example 1-1] except that only hydrazine nitrate (20 g) was used as the high-energy substance.

  The PL intensity of the inorganic compound thus produced (Comparative Example 1-1) was measured by the same method as [Example 1-1] described above. The result is shown in FIG. Moreover, the X-ray diffraction peak of the inorganic compound (Comparative Example 1-1) was measured by the same method as in [Example 1-1] described above. The X-ray diffraction results are shown in FIG.

[Comparative Example 1-2]
In [Example 1-1] described above, an inorganic compound (blue phosphor) was produced in the same manner as [Example 1-1] except that TNT (20 g) was used as the high-energy substance.

  The PL intensity of the inorganic compound thus produced (Comparative Example 1-2) was measured by the same method as [Example 1-1] described above. The result is shown in FIG. Moreover, the X-ray-diffraction peak of the inorganic compound (Comparative Example 1-2) was measured by the same method as [Example 1-1] mentioned above. The X-ray diffraction results are shown in FIG.

[Evaluation 1]
<Appearance inspection>
When the inorganic compound produced in the above [Example 1-1] and the inorganic compound produced in each example of the above [Comparative Example 1-1] and [Comparative Example 1-2] were visually observed, The inorganic compound of [1-1] and [Comparative Example 1-1] was white and was not contaminated by carbon. On the other hand, the inorganic compound of [Comparative Example 1-2] was black, and contamination with carbon could be confirmed.

<Luminescence intensity>
From the PL intensity measurement results shown in FIG. 3, when a mixture of hydrazine nitrate and saturated hydrazine (HN / HH) is used as a high-energy substance (Example 1-1), when TNT is used (Comparative Example 1- It can be seen that the emission intensity is about 16 times that of 2). Further, when using a high energy substance (HN) of hydrazine nitrate alone (Comparative Example 1-1), a light emission intensity about 5 times as high as that using TNT (Comparative Example 1-2) can be obtained. I understand. It can also be seen that when saturated hydrazine is mixed with hydrazine nitrate, a higher emission intensity can be obtained than in the case of hydrazine nitrate alone.

  From the above results, it was confirmed that by using a high-energy substance that does not contain carbon, emission absorption due to black contamination of carbon disappears and high emission intensity can be obtained.

<XRD evaluation>
As can be seen from the X-ray diffraction results shown in FIG. 4, in all the inorganic compounds prepared in each of the above [Example 1-1], [Comparative Example 1-1] and [Comparative Example 1-2], An X-ray diffraction peak of zinc (ZnS) appears, and thereby, in all of [Example 1-1], [Comparative example 1-1] and [Comparative example 1-2], an inorganic material based on ZnS It was confirmed that the compound (blue phosphor) was prepared.

However, an X-ray diffraction peak of barium sulfate (BaSO ₄ ) (a peak indicated by a broken line arrow in FIG. 4) is used for an inorganic compound (Comparative Example 1-1) prepared using a high-energy substance (HN) of hydrazine nitrate alone. It was confirmed that barium sulfate, which is a reaction by-product during the heat treatment (doping treatment), was produced.

[Example 2-1]
An inorganic compound was produced under the same conditions and treatment as in [Example 1-1] described above. That is, as a high energy substance, a mixture of hydrazine nitrate 63.5% by weight and saturated hydrazine 36.5% by weight (HN: HH = 63.5: 36.5 oxygen balance = 1-18% 20 g) An inorganic compound was prepared using The X-ray diffraction peak of the thus produced inorganic compound [Example 2-1] was measured by the same method as [Example 1-1]. The X-ray diffraction results are shown in FIG.

[Example 2-2]
In [Example 1-1] described above, as a high-energy substance, a mixture of hydrazine nitrate 55.0% by weight and saturated hydrazine 45.0% by weight (HN: HH = 55.0: 45.0 oxygen) An inorganic compound was produced in the same manner as in [Example 1-1] except that balance = −24.1% 20 g) was used. The X-ray diffraction peak of the thus produced inorganic compound [Example 2-2] was measured by the same method as [Example 1-1]. The X-ray diffraction results are shown in FIG.

[Comparative Example 2-1]
In the above [Example 1-1], except that a high energy substance (HN: HH = 100: 0 oxygen balance = + 8.4% 20 g) having a hydrazine nitrate weight ratio of 100% by weight was used, Inorganic compounds were prepared as in Example 1-1]. The X-ray diffraction peak of the inorganic compound thus produced [Comparative Example 2-1] was measured by the same method as in [Example 1-1]. The X-ray diffraction results are shown in FIG.

[Evaluation 2]
From the X-ray diffraction results shown in FIG. 5, X-ray diffraction of the inorganic compound (blue phosphor) prepared in [Comparative Example 2-1] (inorganic compound prepared using a high-energy substance (HN) of hydrazine nitrate alone). In the peak, a barium sulfate (BaSO ₄ ) peak (a peak indicated by a broken line arrow in FIG. 5) appears, and barium sulfate which is a reaction by-product in the heat treatment (doping treatment) is mixed. I understand that. In contrast, X-ray diffraction of the inorganic compound (blue phosphor) (inorganic compound prepared using a high energy substance (HN / HH)) prepared in [Example 2-1] and [Example 2-2]. In any of the peaks, no barium sulfate (BaSO ₄ ) peak appears, and it can be seen that no barium sulfate is present.

[Evaluation 3]
The inorganic compound (blue phosphor) produced in [Comparative Example 2-1] was formed to a thickness of 1000 nm on a glass substrate on which an ITO transparent electrode was formed to produce a light emitting layer. An EB vapor deposition apparatus was used as the film forming apparatus. The film forming conditions were such that the degree of vacuum in the vapor deposition chamber was 8 × 10 ⁻⁶ Torr (1.1 × 10 ⁻³ Pa) and the temperature of the glass substrate was 300 ° C. After the film formation, an annealing treatment was performed at a temperature of 600 ° C. for 1 hour in order to improve the crystallinity of the light emitting layer.

When the X-ray diffraction peak was measured for the light emitting layer (deposited film) produced by such treatment by the same method as in [Example 1], a barium sulfate (BaSO ₄ ) peak appeared. On the other hand, the inorganic compound (blue phosphor) produced in [Example 2-1] and [Example 2-2] was formed to a thickness of 1000 nm on the ITO transparent electrode under the same conditions to produce a light emitting layer, When X-ray diffraction peaks were measured by the same method as in [Example 1], no barium sulfate (BaSO ₄ ) peak appeared.

From the above results (XRD evaluation), by making the oxygen balance of the high-energy substance negative, the produced inorganic compound (blue phosphor) and the light-emitting layer formed using the inorganic compound are reacted by-products. It was confirmed that was not generated.
[Summary]
From the above examples and comparative examples, an inorganic compound (inorganic phosphor) is produced using hydrazine nitrate not containing carbon as a high-energy substance that applies high temperature and high pressure to an inorganic composition (containing a compound semiconductor). Thus, it was confirmed that the emission intensity of the inorganic compound was significantly improved as compared with the case of using TNT containing carbon.

  In addition, when a high-energy substance consisting of hydrazine nitrate alone is used, the oxygen balance of the high-energy substance is positive, and the atmosphere during the heat treatment (atmosphere in the sealed container) becomes an oxygen atmosphere. Product (barium sulfate) is produced. On the other hand, by mixing saturated hydrazine with hydrazine nitrate and selecting the mixing ratio to make the oxygen balance of the high-energy substance negative (by making the atmosphere during heat treatment a reducing atmosphere), a reaction by-product It was confirmed that an inorganic compound (inorganic phosphor) free from any product can be produced.

  Therefore, by producing an inorganic compound (inorganic phosphor) using the production method of the present invention, it is possible to obtain an inorganic compound having high emission intensity and free of reaction by-products (impurities). Furthermore, since no reaction by-product is present in the inorganic compound, it is possible to stably perform a film formation process (evaporation or the like) at the time of manufacturing the EL element, and the inorganic EL element can be produced efficiently.

  The present invention can be effectively used to improve the emission intensity of an inorganic compound (inorganic phosphor) used for manufacturing an inorganic EL element.

DESCRIPTION OF SYMBOLS 1 Stainless steel sealed container 11 Container body 12 Lid 13 Hexagon socket head cap screw 2 Heating furnace 3 Gas burner M Raw material (inorganic composition)
E High energy materials

Claims (2)

A method for producing an inorganic compound used for producing an inorganic EL element,
An inorganic composition containing a compound semiconductor and a high energy substance mixed with hydrazine nitrate and saturated hydrazine sealed in a sealed container, and the high energy substance in the sealed container is thermally decomposed by heating. A method for producing an inorganic compound. In the manufacturing method of the inorganic compound of Claim 1,
The mixing ratio of the high energy substance hydrazine nitrate and saturated hydrazine is set so that the atmosphere in the sealed container when the high energy substance is thermally decomposed in the sealed container is a reducing atmosphere. A method for producing an inorganic compound.

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