CN103415486A - Process for producing sintered magnesium oxide material - Google Patents
Process for producing sintered magnesium oxide material Download PDFInfo
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- CN103415486A CN103415486A CN2012800116524A CN201280011652A CN103415486A CN 103415486 A CN103415486 A CN 103415486A CN 2012800116524 A CN2012800116524 A CN 2012800116524A CN 201280011652 A CN201280011652 A CN 201280011652A CN 103415486 A CN103415486 A CN 103415486A
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
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- C01F5/00—Compounds of magnesium
- C01F5/02—Magnesia
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- C04B35/03—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on magnesium oxide, calcium oxide or oxide mixtures derived from dolomite
- C04B35/04—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on magnesium oxide, calcium oxide or oxide mixtures derived from dolomite based on magnesium oxide
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- C04B35/62605—Treating the starting powders individually or as mixtures
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- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
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- H01J11/20—Constructional details
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- C04B2235/3205—Alkaline earth oxides or oxide forming salts thereof, e.g. beryllium oxide
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Abstract
Provided is a production process which can produce a sintered magnesium oxide material containing magnesium oxide, calcium oxide and aluminum and having a sufficiently high sintered density from a magnesium oxide precursor in which aluminum is dispersed uniformly. A process for producing a sintered magnesium oxide material containing magnesium oxide, calcium oxide and aluminum. In the process, firstly, a magnesium hydroxide slurry containing aluminum is prepared, the magnesium hydroxide slurry is subjected to a hydrothermal treatment, the treatment product is subjected to filtering, washing with water and drying to produce magnesium hydroxide particles, and the magnesium hydroxide particles are fired, thereby producing magnesium oxide particles. Next, the magnesium oxide particles are mixed with calcium compound particles and a binder, the mixture is granulated to produce a granulated powder, the granulated powder is molded in a mold to produce a molding, and the molding is sintered, thereby producing the sintered material.
Description
Technical field
The present invention relates to be suitable as and can form plasma panel (hereinafter referred to as PDP(Plasma Display Panel)) the manufacture method of magnesium oxide sinter of deposition material of protective membrane.
Background technology
PDP is a plurality of airtight small discharge spaces are set in the gap of two glass substrates display unit.For example, in the PDP of matrix display mode, a plurality of electrodes are arranged with reticulation, and make the discharge cell of cross part of each electrode optionally luminous and show image.At the AC(Alternating of representational surface discharge type Current; Interchange) in type PDP, the show electrode of front panel is covered by dielectric layer, forms protective membrane on this external dielectric layer.Protective membrane is to have to prevent that dielectric layer surface in direct electric discharge changes and the function of the situation that discharge inception voltage rises because dielectric layer is exposed to, and demonstrates the layer of the characteristic that can not change because of the sputter of ion bombardment.
Current, the protective membrane that PDP uses normally is formed on dielectric substance by the means of electron beam deposition of the sintered compact using magnesium oxide etc. as target.Yet in order to make further economize on electricity and require further to reduce discharge inception voltage of PDP, the protective membrane of using as PDP requires to have the low discharge starting voltage, secondary electron yield is high, to the material of sputter tolerance.
From the viewpoint, in patent documentation 1, put down in writing and utilized the metal oxide formed by magnesium oxide and calcium oxide to form and contain the protective membrane of aluminium.In the document, put down in writing and in the protective membrane of principal constituent, contained calcium oxide take magnesium oxide, can bring into play good secondary electron emission characteristic with this, can reduce discharge inception voltage.In addition, put down in writing when the calcium oxide in protective membrane and carbonic acid gas are combined into calcium carbonate, the effect that discharge inception voltage reduces weakens, and, by adding aluminium, can suppress by the variation of calcium oxide to calcium carbonate, can suppress the rising of discharge inception voltage.
The deposition material, the magnesium oxide sinter that comprise magnesium oxide and calcium oxide that use when forming such protective membrane are disclosed in patent documentation 2 and patent documentation 3.
In patent documentation 2 and patent documentation 3, put down in writing the manufacture method as this sintered compact, make the powder of magnesium oxide powder, calcium oxide or calcium oxide presoma and binding agent blending dispersion and prepare slurry in aqueous dispersion medium, utilize the described slurry of spray-dryer spraying drying to obtain granules with this, at in-mold molding, and the forming composition that will obtain is burnt till and obtains sintered compact by granules.
Especially in patent documentation 3, disclose and further utilized the aluminum compound particle, obtained containing the magnesium oxide sinter of magnesium oxide, calcium oxide and aluminium.
The prior art document:
Patent documentation:
Patent documentation 1: TOHKEMY 2010-140837 communique;
Patent documentation 2: TOHKEMY 2005-330574 communique;
Patent documentation 3: TOHKEMY 2010-143798 communique.
Summary of the invention
The problem that invention will solve:
Yet, at the magnesium oxide particle of the aluminum compound particle by by the solid as disclosed in patent documentation 3 and solid and during calcium cpd mixes and sintering manufactures the method for sintered compact, aluminium can not fully obtain the effect as sintering aid in the particle surface segregation, especially when increasing the proportioning of calcium oxide, can only obtain the sintered compact that sintered density is low.In the operation that forms the protective membrane that PDP uses, when deposition material is used, there is the problem that becomes the reason that splash occurs in the sintered compact that such sintered density is low.
In order to pass through the sintered compact of the accomplished sufficient sintered density of aforesaid method; and need to increase the aluminium content in sintered compact, but by the protective membrane that the sintered compact that comprises a large amount of aluminium forms, can be reduced the effect (paragraph of patent documentation 1 [0097]～[0100], reach Fig. 7) of the rising that suppresses discharge inception voltage.
Again; by the sintered compact that aforesaid method obtains, aluminium is segregation in sintered compact, and using such sintered compact when deposition material is used and form protective membrane; aluminium is also segregation in the protective membrane obtained, the effect of the rising of the discharge inception voltage that therefore can not fully be inhibited.
The present invention is in view of above-mentioned present situation, even its objective is, provides and can manufacture also sufficiently high, the manufacture method that contains the magnesium oxide sinter of magnesium oxide, calcium oxide and aluminium of the few sintered density of addition that the aluminium contained disperses aluminium equably.
The means of dealing with problems:
The inventor finds after deliberation, in manufacture, contain magnesium oxide, during the magnesium oxide sinter of calcium oxide and aluminium, in the process of manufacture as the magnesium hydroxide of magnesian precursor, for aluminium is disperseed equably, and in the aqueous solution that contains magnesium or magnesium hydroxide slurry, add in advance aluminum compound, obtain containing the magnesium hydroxide of aluminium, the magnesium oxide particle that contains aluminium and calcium oxide or its precursor that will be obtained by this magnesium hydroxide afterwards, and binding agent mixes, granulation, moulding and burning till, with this, obtaining aluminium disperses equably, even if the few sintered density of the addition of aluminium is sufficiently high sintered compact also, thereby reached the present invention.
That is, the manufacture method of magnesium oxide sinter of the present invention is to manufacture the method for the magnesium oxide sinter that contains magnesium oxide, calcium oxide and aluminium, comprises: preparation contains the operation (A) of the magnesium hydroxide slurry of aluminium; Described magnesium hydroxide slurry is carried out to the operation (B) of hydrothermal treatment consists; To through the described magnesium hydroxide slurry of hydrothermal treatment consists, filter, wash and drying, obtain the operation (C) of magnesium hydroxide particle; Burn till described magnesium hydroxide particle, obtain the operation (D) of magnesium oxide particle; By described magnesium oxide particle, calcium cpd particle and binding agent mixes and granulation, obtain the operation (E) of prilling powder; Described prilling powder moulding is formed to the operation (F) of formed body in mould; And the operation of the described formed body of sintering (G).
The invention effect:
According to the manufacture method of magnesium oxide sinter of the present invention, the few sintered density of addition that aluminium in sintered compact disperses aluminium equably even if can be manufactured on is sufficiently high, the magnesium oxide sinter that contains magnesium oxide, calcium oxide and aluminium also.
Even the magnesium oxide sinter obtained thus is in the situation that to improve the proportioning sintered density of calcium oxide also enough high, so as deposition material, use and while forming protective membrane the generation of the splash in the time of can suppressing to deposit.Again, the addition of aluminium is few, and aluminium can segregation in the protective membrane obtained, and therefore can form the sufficient protective membrane of inhibition of the rising of discharge inception voltage.
Embodiment
The constituent of the magnesium oxide sinter by manufacture of the present invention be take magnesium oxide as main body (contained with the ratio more than 50 quality % in total amount), contains in addition calcium oxide and aluminium.Now, this aluminium both can exist with the state of metallic aluminium or aluminum oxide, also can be solid-solubilized in other elements.Sintered compact refers to the aggregate of particle heated to (sintering) with the temperature lower than fusing point, with the growth of this solid phase diffusion by powder, neck, the movement of crystal boundary etc., connects between particle and the formed body of the densification of manufacturing.
The content of the calcium oxide in the magnesium oxide sinter of manufacturing is 2～49.9 quality %.When being less than 2 quality %, the effect that reduces discharge inception voltage by the protective membrane for PDP that uses described sintered compact to form as deposition material is insufficient, when surpassing 49.9 quality %, splash occurs easily during film forming.2～30 quality % preferably.
The content of the aluminium in the magnesium oxide sinter of manufacturing is 0.001～1 quality %.When being less than 0.001 quality %; sintered density is insufficient; therefore splash easily occurs when film forming, when surpassing 1 quality %, the effect that suppresses the rising of discharge inception voltage by the protective membrane for PDP that uses described sintered compact to form as deposition material can descend.0.004～0.2 quality % preferably.
Manufacturing method according to the invention, can manufacture sintered density and be more than 95%, preferably more than 96%, more preferably more than 97%, the sintered compact more than 98% further preferably.Like this, owing to being the sintered compact that sintered density is very high, thereby, when the deposition material using this sintered compact as means of electron beam deposition, in the vacuum deposition method of ion plating method or sputtering method etc. is used and carries out film forming, can suppress the generation of splash.
Below with the manufacture method of each specification magnesium oxide sinter of the present invention.
(preparation contains the operation of the aqueous solution of magnesium)
At first, be formulated in the aqueous solution that contains magnesium used in operation (A).The aqueous solution that contains magnesium is not particularly limited, for example can enumerate contain from the group who is formed by chlorate, nitrate, vitriol, carbonate, acetate and oxalate, select at least a more than the aqueous solution.In order to be reduced the magnesium oxide particle of aluminium impurity in addition, be preferably magnesium chloride brine.
Below, specifically describe the operation of the situation of having used magnesium chloride brine, but be not limited to this.The concentration of the magnesium chloride brine of preparation is preferably 0.1～10mol/L.When concentration is less than 0.1mol/L, the production efficiency variation.Again, when concentration during higher than 10mol/L, the viscosity increased of magnesium hydroxide slurry, treatability variation.The concentration of magnesium chloride brine is preferably 0.5～5mol/L.
At first, prepare magnesium chloride brine.For example, highly purified magnesium chloride more than purity 99 quality % is (as magnesium chloride, can use magnesium chloride hexahydrate or Magnesium Chloride Anhydrous or seawater, buck or bittern) in add pure water and (pass through ion exchange resin, refining water till making specific conductivity reach below 0.1 μ S/cm), with this, can be used as magnesium chloride brine.The concentration of magnesium chloride brine can be 0.1～10mol/L, is preferably 0.5～5mol/L.
(preparation process (A) that contains the magnesium hydroxide slurry of aluminium)
The magnesium hydroxide slurry that contains the aluminium of specified amount is prepared by following operation A-1 or operation A-2.
(operation A-1 adds the situation of aluminum compound in containing the aqueous solution of magnesium)
The aluminum compound of specified amount is added and to be mixed in the aqueous solution that contains magnesium, so that contained aluminium reaches the scope of 0.001～1 quality % in the magnesium oxide sinter obtained.The aluminum compound added is not particularly limited, for example can enumerate contain from the group who is formed by chlorate, nitrate, carbonate, acetate and oxalate, select at least a more than compound.For example, in order to be reduced the magnesium hydroxide slurry of the impurity beyond aluminium, when using magnesium chloride brine, as aluminum compound aluminum chloride hexahydrate preferably.Again, because of same reason, more than the purity of aluminum compound is preferably 99.9 quality %.
In the resulting aqueous solution that contains magnesium that contains aluminium, add alkaline aqueous solution, obtain containing the magnesium hydroxide slurry of aluminium.The alkaline aqueous solution used is not particularly limited, as example can enumerate contain from the group that sodium hydroxide, calcium hydroxide, ammonium salt form, select at least a more than the aqueous solution.The concentration of alkaline aqueous solution is preferably 1～18mol/L.When the concentration of alkaline aqueous solution is less than 1mol/L, the production efficiency variation.Again, when concentration during higher than 18mol/L, the viscosity increased of magnesium hydroxide slurry, treatability variation.The concentration of 4～18mol/L preferably.Contain the aqueous solution of magnesium and the reactivity of alkaline aqueous solution and be preferably 85～98mol%.Here, reactivity refers to the whole magnesium compound contained in the aqueous solution of magnesium is converted into when the required alkali number of magnesium hydroxide is 100mol% to the value calculated.When reactivity is less than 85mol%, the production efficiency variation.Again, during higher than 98mol%, the impurity of slurry can increase when reactivity.
(operation A-2 adds the situation of aluminum compound in magnesium hydroxide slurry)
In containing the aqueous solution of magnesium, add alkaline aqueous solution, obtain magnesium hydroxide slurry.The kind of the alkaline aqueous solution used and concentration and reactivity also can be identical with operation A-1.In resulting magnesium hydroxide slurry, add the quantitative aluminum compound of hybrid regulatory so that in the magnesium oxide sinter obtained contained aluminium reach the scope of 0.001～1 quality %, thereby obtain containing the magnesium hydroxide slurry of aluminium.Kind and the purity of the aluminum compound used also can be identical with operation A-1.
(operation of hydrothermal treatment consists magnesium hydroxide slurry (B))
The resulting magnesium hydroxide slurry of hydrothermal treatment consists, thus the magnesium hydroxide slurry that hydrothermal treatment consists is crossed obtained.
Hydrothermal treatment consists can be by magnesium hydroxide slurry for example being used autoclave under 101 ℃～200 ℃, keep while stirring carrying out.During lower than 101 ℃, crystallization is not grown when the hydrothermal treatment consists temperature, and produces flocculated particle and dispersed variation.Again, when hydrothermal treatment consists temperature crystallization hypertrophy during higher than 200 ℃, the tendency that exists particle diameter excessively to increase.The hydrothermal treatment consists temperature is preferably 105 ℃～150 ℃.The hydrothermal treatment consists time can be 0.5～5 hour.When the hydrothermal treatment consists time is this scope, crystalline growth and particle diameter can be controlled in suitable scope.The hydrothermal treatment consists time is preferably 1～2 hour.
(obtaining the operation (C) of magnesium hydroxide particle)
The magnesium hydroxide slurry that hydrothermal treatment consists is crossed filters, washing and drying treatment, obtains magnesium hydroxide particle with this.
Washing can be to drop into afterwards and take quality and with respect to dry hydrogen magnesium oxide, carry out as 5～100 times, the pure water that is preferably 20～50 times as benchmark in filtration.
(obtaining the operation (D) of magnesium oxide particle)
By burning till above-mentioned magnesium hydroxide particle, thereby obtain magnesium oxide particle.Concrete is, by magnesium hydroxide particle for example in atmospheric atmosphere the heat-up rate (being preferably 3～10 ℃/minute) with 1～20 ℃/minute be warming up to 500 ℃～1600 ℃, be preferably 600～1000 ℃, after intensification, 500 ℃～1600 ℃, be preferably under 600～1000 ℃ and burnt till 0.1～5 hour, with this, can obtain magnesium oxide particle.For the protective membrane that makes to sneak into plasma display is enough few with the metallic impurity in deposition material, it is more than 99.9 quality % that the purity of the magnesium oxide particle obtained is preferably removed the purity that aluminium calculates, more preferably more than 99.95 quality %.
(mixing and granulating working procedure (E))
Then, to above-mentioned magnesium oxide particle blending calcium compound particle and binding agent granulation, obtain prilling powder.Prilling process does not limit, and can utilize and rotate comminution granulation and spray granulation etc.
As above-mentioned calcium cpd, be not particularly limited, for example can use calcium carbonate, calcium hydroxide, calcium oxide.The purity of these calcium cpds is more than 99 quality %, more than being preferably 99.9 quality %.Again, the median size of calcium cpd is preferably the scope of 0.01～15 μ m.Above-mentioned calcium cpd particle is as long as the calcium oxide of use in the magnesium oxide sinter of manufacturing reaches the amount of the amount of hope.
As above-mentioned binding agent, be not particularly limited, for example can enumerate CMC(carboxy methyl cellulose; Carboxymethyl cellulose) etc. derivatived cellulose, PVA(Poly vinyl alcohol; Polyvinyl alcohol), acrylic resin, vinyl acetate between to for plastic are resin etc.As its usage quantity, with solid substance, count 1～10 mass parts left and right with respect to summation 100 mass parts of the amount of powder that is scaled oxide compound.Binding agent is preferably used as binder solution, and the concentration of this solution is 5～50 quality % left and right preferably.In addition, also can together with binding agent, share the additive of dispersion agent etc.
(molding procedure (F))
Described granulation body be directed in the mould of regulation and carry out moulding by pressurizing device, forming formed body.
Pressurizing device and mould are not particularly limited; can be used as particularly press and the mould that for the film formed target of the protection of used for plasma display screen, can be shaped to necessary shape and size (for example, disk, cylinder and the prism-shaped etc. of thickness 3.0mm left and right).Pressurizing device for example can use the single shaft pressurizing device.In order to regulate the relative density of the formed body obtained, moulding pressure for example preferably is set as 50～600MPa.
The thickness of the formed body by the moulding of press applied pressure can be 0.1～10.0mm.If the thickness of formed body is such value, can carry out preferably sintering, again, the sintered compact that can obtain after sintering finishes is used preferably as target.
(firing process (G))
By burning till resulting formed body, can obtain as target compound, magnesium oxide sinter that contain magnesium oxide, calcium oxide and aluminium.When burning till, can use electric furnace, steam stove etc.For the firing temperature that obtains highdensity sintered compact, be 1200～2400 ℃, be preferably 1300～1800 ℃.Again, firing time is 0.5～20 hour, is preferably 5～15 hours.Burn till and can under the easy to handle atmospheric atmosphere, carry out.Also can in nitrogen atmosphere or in atmosphere of inert gases in addition, carry out as required again.
The magnesium oxide sinter obtained in the present invention can be suitable as the deposition material utilization of using when forming the protective membrane of plasma panel by vacuum deposition method.Vacuum deposition method is not particularly limited, and can use means of electron beam deposition, ion plating method, sputtering method etc.
Embodiment
Below exemplify embodiment and further describe the present invention, but the present invention is not limited to these embodiment.
(analytical procedure)
Measure by the following method the physical properties of resulting sintered compact.
(1) content assaying method of aluminium element and impurity element
For the element as determination object (Ag, Al, B, Ba, Bi, Cd, Co, Cr, Cu, Fe, Ga, In, K, Li, Mn, Mo, Na, Ni, P, Pb, S, Si, Sr, Tl, V, Zn, Ti and Zr), use ICP apparatus for analyzing luminosity (trade name: SPS-5100, Seiko Instruments Inc. manufactures), after being dissolved in to acid, test portion measured quality.
(2) method for detecting purity
For the purity of magnesium oxide particle, calculate as the value of the summation of the quality that deducts the impurity element except aluminium of measuring by above-mentioned " content assaying method of aluminium element and impurity element " from 100 quality %.
(3) content assaying method of calcium oxide
Use automatic titration device (COMTITE-980, flat natural pond industry is manufactured), measured the calcium oxide content contained in the sintered compact.
(4) calculation method of the relative density of sintered compact (sintered density)
The relative density of sintered compact is obtained by Archimedes's method.But, using magnesian theoretical density as 3.58g/cc, using the theoretical density of calcium oxide as 3.32g/cc, the theoretical density of aluminum oxide is calculated as 3.97g/cc.
(5) laser diffraction and scattering formula particle size distribution
Use laser diffraction and scattering formula particle size distribution device (trade name: MT3300, day machine dress company manufactures) to measure accumulative total 50% particle diameter (D50) of volume reference.
(embodiment 1)
(preparing the operation of magnesium chloride brine)
As magnesium chloride, prepared that purity 99 quality % are above, the aqueous solution of concentration 3.5mol/L.In this magnesium chloride brine, add pure water (be refined to specific conductivity by ion exchange resin and reach the water below 0.1 μ s/cm), regulate concentration with this, obtain the magnesium chloride brine of concentration 2.0mol/L.
(operation A)
Aluminum chloride hexahydrate (high-purity chemical institute of Co., Ltd. manufacture: more than purity 99.9 quality %) is added and is mixed in magnesium chloride brine with the amount of the aluminium that can contain 500 quality ppm in sintered compact.The aqueous sodium hydroxide solution that is 15mol/L by the magnesium chloride brine that contains aluminium that obtains and concentration reacts so that the reactivity of magnesium chloride reaches 95mol%, thereby compound concentration is the magnesium hydroxide slurry that contains aluminium of 100g/L.
(process B)
Use autoclave to keep while stirring 1 hour under 150 ℃ the magnesium hydroxide slurry obtained, carry out hydrothermal treatment consists (heated and stirred processing) with this.
(operation C)
The magnesium hydroxide slurry that filtered water is heat treated, obtain the magnesium hydroxide filter cake by washing.Filtration drop into afterwards take quality as benchmark with respect to the pure water of dry hydrogen magnesium oxide as 40 times, with this, wash.The pulverizing of magnesium hydroxide filter cake, drying by obtaining, obtain magnesium hydroxide particle.
(step D)
The magnesium hydroxide particle that obtains, under atmospheric atmosphere, was burnt till 1 hour under 1000 ℃, obtain magnesium oxide particle with this.
(operation E)
With respect to magnesium oxide particle 100 mass parts that obtain, (Kanto Kagaku K. K. manufactures to add calcium carbonate, purity: more than 99.99 quality %, D50:12 μ m) 9 mass parts (convert and be equivalent to contain the amount of 5 quality % in sintered compact with calcium oxide), and as the carboxy methyl cellulose of the derivatived cellulose of binding agent, make this carboxy methyl cellulose in solid substance, reach 4 mass parts with respect to summation 100 mass parts of magnesium oxide particle and calcium carbonate granule, and mixing and granulation.
(operation F)
After the granulation soma obtained is dry, by extrusion forming (forming pressure: 300MPa) be shaped to the rectangular-shaped of 8mm * 8mm * 3.5mm, obtain formed body.
(operation G)
The formed body obtained was burnt till 6 hours in electric furnace, obtain containing the sintered compact of magnesium oxide, calcium oxide and aluminium under 1650 ℃.
(embodiment 2)
At first, with embodiment 1, obtain in the same manner magnesium chloride brine.
Then, in (operation A), by concentration, be the aqueous sodium hydroxide solution of 15mol/L and magnesium chloride brine so that the reactivity of magnesium chloride reaches the degree of 95mol% reacts, thereby prepared concentration, be the magnesium hydroxide slurry of 100g/L.And then, aluminum chloride hexahydrate (high-purity chemical institute of Co., Ltd. manufacture: more than purity 99.9 quality %) is added and is mixed in the magnesium hydroxide slurry obtained with the amount of the aluminium that can contain 500 quality ppm in sintered compact, obtain containing the magnesium hydroxide slurry of aluminium with this.
Then, carry out in the same manner (process B)～(operation G) with embodiment 1, obtain containing the sintered compact of magnesium oxide, calcium oxide and aluminium.
(embodiment 3)
Make the aluminium amount in sintered compact reach 100 quality ppm ground interpolation aluminum chloride hexahydrates, and interpolation calcium carbonate, make the addition of calcium carbonate for calcium oxide, converting and be equivalent to contain the amount of 2 quality % in sintered compact, with embodiment 2, carry out in the same manner in addition, obtain containing the sintered compact of magnesium oxide, calcium oxide and aluminium.
(embodiment 4)
Make the aluminium amount in sintered compact reach 200 quality ppm ground interpolation aluminum chloride hexahydrates, and interpolation calcium carbonate, make the addition of calcium carbonate for calcium oxide, converting and be equivalent to contain the amount of 5 quality % in sintered compact, with embodiment 2, carry out in the same manner in addition, obtain containing the sintered compact of magnesium oxide, calcium oxide and aluminium.
(embodiment 5)
Make the aluminium amount in sintered compact reach 300 quality ppm ground interpolation aluminum chloride hexahydrates, and interpolation calcium carbonate, make the addition of calcium carbonate for calcium oxide, converting and be equivalent to contain the amount of 5 quality % in sintered compact, with embodiment 2, carry out in the same manner in addition, obtain containing the sintered compact of magnesium oxide, calcium oxide and aluminium.
(embodiment 6)
Make the aluminium amount in sintered compact reach 200 quality ppm ground interpolation aluminum chloride hexahydrates, and interpolation calcium carbonate, make the addition of calcium carbonate for calcium oxide, converting and be equivalent to contain the amount of 10 quality % in sintered compact, with embodiment 2, carry out in the same manner in addition, obtain containing the sintered compact of magnesium oxide, calcium oxide and aluminium.
(embodiment 7)
Make the aluminium amount in sintered compact reach 500 quality ppm ground interpolation aluminum chloride hexahydrates, and interpolation calcium carbonate, make the addition of calcium carbonate for calcium oxide, converting and be equivalent to contain the amount of 10 quality % in sintered compact, with embodiment 2, carry out in the same manner in addition, obtain containing the sintered compact of magnesium oxide, calcium oxide and aluminium.
(embodiment 8)
Make the aluminium amount in sintered compact reach 1000 quality ppm ground interpolation aluminum chloride hexahydrates, and interpolation calcium carbonate, make the addition of calcium carbonate for calcium oxide, converting and be equivalent to contain the amount of 15 quality % in sintered compact, with embodiment 2, carry out in the same manner in addition, obtain containing the sintered compact of magnesium oxide, calcium oxide and aluminium.
(embodiment 9)
Make the aluminium amount in sintered compact reach 2000 quality ppm ground interpolation aluminum chloride hexahydrates, and interpolation calcium carbonate, make the addition of calcium carbonate for calcium oxide, converting and be equivalent to contain the amount of 30 quality % in sintered compact, with embodiment 2, carry out in the same manner in addition, obtain containing the sintered compact of magnesium oxide, calcium oxide and aluminium.
(embodiment 10)
Make the aluminium amount in sintered compact reach 40 quality ppm ground interpolation aluminum chloride hexahydrates, further making the calcium cpd added is that (Kanto Kagaku K. K. manufactures calcium hydroxide, purity: more than 99.9 quality %, D50:12 μ m), make the addition of calcium hydroxide for calcium oxide, converting and be equivalent to contain the amount of 2 quality % in sintered compact, with embodiment 2, carry out in the same manner in addition, obtain containing the sintered compact of magnesium oxide, calcium oxide and aluminium.
(embodiment 11)
Making the calcium cpd added is that (Kanto Kagaku K. K. manufactures calcium hydroxide, purity: more than 99.9 quality %, D50:12 μ m), make the addition of calcium hydroxide for calcium oxide, converting and be equivalent to contain the amount of 5 quality % in sintered compact, with embodiment 2, carry out in the same manner in addition, obtain containing the sintered compact of magnesium oxide, calcium oxide and aluminium.
(embodiment 12)
Making the calcium cpd added is that (Kanto Kagaku K. K. manufactures calcium oxide, purity: more than 99.9 quality %, D50:15 μ m), making its addition is the amount that is equivalent to contain 5 quality % in sintered compact, with embodiment 2, carry out in the same manner in addition, obtain containing the sintered compact of magnesium oxide, calcium oxide and aluminium.
(embodiment 13)
Making the aluminum compound added is aluminum nitrate nonahydrate (high-purity chemical institute of Co., Ltd. manufactures, purity: more than 99.9 quality %), with embodiment 2, carries out in the same manner in addition, obtains containing the sintered compact of magnesium oxide, calcium oxide and aluminium.
(embodiment 14)
Making the aluminum compound added is Tai-Ace S 150 (high-purity chemical institute of Co., Ltd. manufactures, purity: more than 99.9 quality %), with embodiment 2, carries out in the same manner in addition, obtains containing the sintered compact of magnesium oxide, calcium oxide and aluminium.
(comparative example 1)
With embodiment 1, obtain in the same manner magnesium chloride brine.
Then, do not carry out (operation A), react and make the reactivity of magnesium chloride reach aqueous sodium hydroxide solution and the magnesium chloride brine that 95mol% ground is 15mol/L by concentration, having prepared concentration is the magnesium hydroxide slurry of 100g/L.
Then, with embodiment 1, carried out in the same manner (process B)～(step D).
Then, in (operation E), make with respect to magnesium oxide particle 100 mass parts that obtain, aluminium content in sintered compact reaches 500 quality ppm ground and adds aluminum oxide (high-purity chemical institute of Co., Ltd. manufacture, more than purity 99.9 quality %), (Kanto Kagaku K. K. manufactures, purity: more than 99.9 quality % further to add calcium carbonate, D50:12 μ m) 9 mass parts (convert and be equivalent to contain the amount of 5 quality % in sintered compact with calcium oxide) and binding agent, and mixing, granulation.
Then, carry out in the same manner (operation F) and (operation G) with embodiment 1, obtain containing the sintered compact of magnesium oxide, calcium oxide and aluminium.
(comparative example 2)
Make the aluminium content in sintered compact reach 100 quality ppm ground interpolation aluminum oxide, calcium carbonate is equivalent to contain the amount interpolation of 2 quality % in sintered compact by with calcium oxide, converting, with comparative example 1, carry out in the same manner in addition, obtain containing the sintered compact of magnesium oxide, calcium oxide and aluminium.
(comparative example 3)
Make the aluminium content in sintered compact reach 500 quality ppm ground interpolation aluminum oxide, calcium carbonate is equivalent to contain the amount interpolation of 10 quality % in sintered compact by with calcium oxide, converting, with comparative example 1, carry out in the same manner in addition, obtain containing the sintered compact of magnesium oxide, calcium oxide and aluminium.
(comparative example 4)
Make the aluminium content in sintered compact reach 1000 quality ppm ground interpolation aluminum oxide, calcium carbonate is equivalent to contain the amount interpolation of 15 quality % in sintered compact by with calcium oxide, converting, with comparative example 1, carry out in the same manner in addition, obtain containing the sintered compact of magnesium oxide, calcium oxide and aluminium.
Below be illustrated in the physical properties of the sintered compact that contains magnesium oxide, calcium oxide and aluminium obtained in above embodiment and comparative example.
[table 1]
As can be known by table 1, in embodiment 1～14, can access the sintered compact that aluminium disperses equably in sintered compact, sintered density is high.
Claims (14)
1. a manufacture method that contains the magnesium oxide sinter of magnesium oxide, calcium oxide and aluminium, be the method for manufacturing the magnesium oxide sinter that contains magnesium oxide, calcium oxide and aluminium, comprising:
Preparation contains the operation (A) of the magnesium hydroxide slurry of aluminium;
Described magnesium hydroxide slurry is carried out to the operation (B) of hydrothermal treatment consists;
To through the described magnesium hydroxide slurry of hydrothermal treatment consists, filter, wash and drying, obtain the operation (C) of magnesium hydroxide particle;
Burn till described magnesium hydroxide particle, obtain the operation (D) of magnesium oxide particle;
By described magnesium oxide particle, calcium cpd particle and binding agent mixes and granulation, obtain the operation (E) of prilling powder;
Described prilling powder moulding is formed to the operation (F) of formed body in mould; And
The operation of the described formed body of sintering (G).
2. the manufacture method of magnesium oxide sinter according to claim 1, is characterized in that, described magnesium oxide sinter contains that magnesium oxide 50 quality % are above, calcium oxide 2～49.9 quality % and aluminium 0.001～1 quality %.
3. the manufacture method of magnesium oxide sinter according to claim 1, is characterized in that, described operation (A) is, after in containing the aqueous solution of magnesium, adding aluminum compound, to react with alkaline aqueous solution, prepares the described magnesium hydroxide slurry that contains aluminium with this.
4. the manufacture method of magnesium oxide sinter according to claim 1, is characterized in that, described operation (A) be at the aqueous solution that makes to contain magnesium with after alkaline aqueous solution reacts, add aluminum compound, with this, prepare the described magnesium hydroxide slurry that contains aluminium.
5. according to the manufacture method of claim 3 or 4 described magnesium oxide sinters, it is characterized in that, described aluminum compound is more than purity 99.9 quality %, and contain from the group who is formed by chlorate, nitrate, vitriol, carbonate, acetate and oxalate, select at least a more than compound.
6. according to the manufacture method of claim 3 or 4 described magnesium oxide sinters, it is characterized in that, the described aqueous solution that contains magnesium be contain from the group who is formed by chlorate, nitrate, vitriol, carbonate, acetate and oxalate, select at least a more than the aqueous solution.
7. according to the manufacture method of claim 3 or 4 described magnesium oxide sinters, it is characterized in that, described alkaline aqueous solution be contain from the group who is formed by sodium hydroxide, calcium hydroxide and ammonium salt, select at least a more than the aqueous solution.
8. the manufacture method of magnesium oxide sinter according to claim 1 and 2, it is characterized in that, described calcium cpd particle is more than purity 99.9 quality %, median size is the scope of 0.01～15 μ m, and contain from the group who is formed by calcium carbonate, calcium hydroxide and calcium oxide, select at least a more than compound.
9. according to the manufacture method of claim 3 or 4 described magnesium oxide sinters, it is characterized in that, in described operation (A), to make concentration be scope described of the 0.1～10mol/L aqueous solution that contains magnesium is the scope of 1～18mol/L with concentration described alkaline aqueous solution reacts with reactivity 85～98mol%.
10. the manufacture method of magnesium oxide sinter according to claim 1 and 2, is characterized in that, in described operation (B), makes described magnesium hydroxide slurry at the temperature of the scope of 101～200 ℃, keep 0.5～5 hour Di carrying out hydrothermal treatment consists.
11. the manufacture method of magnesium oxide sinter according to claim 1 and 2, it is characterized in that, in described operation (D), described magnesium hydroxide particle was burnt till 0.1～5 hour at the temperature of the scope of 500～1600 ℃, the purity that the aluminium that is removed is calculated is the above described magnesium oxide particles of 99.9 quality %.
12. the manufacture method of magnesium oxide sinter according to claim 1 and 2; it is characterized in that; in described operation (E); to contain from by derivatived cellulose, acrylic resin and vinyl acetate between to for plastic, being the binding agent more than select in the group that forms of resin at least a, add with the scope that summation 100 mass parts with respect to described magnesium oxide particle and described calcium cpd particle being scaled to oxide compound are counted 1～10 mass parts with solid substance.
13. the manufacture method of magnesium oxide sinter according to claim 1 and 2, is characterized in that, in described operation (F), carries out the moulding of described prilling powder with the forming pressure of the scope of 50～600MPa.
14. the manufacture method of magnesium oxide sinter according to claim 1 and 2, is characterized in that, in described operation (G), described formed body burnt till 0.5～20 hour at the temperature of the scope of 1300～1800 ℃.
Applications Claiming Priority (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2011065711A JP2012201528A (en) | 2011-03-24 | 2011-03-24 | Method for producing magnesium oxide sintered body |
| JP2011-065711 | 2011-03-24 | ||
| PCT/JP2012/000945 WO2012127771A1 (en) | 2011-03-24 | 2012-02-14 | Process for producing sintered magnesium oxide material |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN103415486A true CN103415486A (en) | 2013-11-27 |
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| CN2012800116524A Pending CN103415486A (en) | 2011-03-24 | 2012-02-14 | Process for producing sintered magnesium oxide material |
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| JP (1) | JP2012201528A (en) |
| CN (1) | CN103415486A (en) |
| TW (1) | TW201238929A (en) |
| WO (1) | WO2012127771A1 (en) |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104129807A (en) * | 2014-08-05 | 2014-11-05 | 四川虹欧显示器件有限公司 | Microcrystalline material MgCaO powder, microcrystalline material as well as preparation methods and applications of MgCaO powder and microcrystalline material |
| CN106893976A (en) * | 2017-01-18 | 2017-06-27 | 东莞市佳乾新材料科技有限公司 | A kind of method for preparing MgO film as target with high-purity compact magnesia |
| CN107382283A (en) * | 2017-09-06 | 2017-11-24 | 盐城市华康电热绝缘材料厂 | The dry-pressing preparation method of magnesia ceramics |
| CN111684039A (en) * | 2018-02-16 | 2020-09-18 | 达泰豪化学工业株式会社 | Chemical heat storage material and preparation method thereof |
| JP7470246B1 (en) | 2023-11-29 | 2024-04-17 | セトラスホールディングス株式会社 | Magnesium oxide for annealing separator, its manufacturing method, and manufacturing method of grain-oriented electrical steel sheet using the same |
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| CN1064147A (en) * | 1992-02-13 | 1992-09-02 | 鞍山钢铁公司 | A kind of material used as bottom of sinering furnace |
| JP2000290062A (en) * | 1999-04-05 | 2000-10-17 | Mitsubishi Materials Corp | MgO VAPOR-DEPOSITED MATERIAL AND ITS PRODUCTION |
| JP2009067603A (en) * | 2007-09-10 | 2009-04-02 | Tateho Chem Ind Co Ltd | Magnesium oxide sintered compact |
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| JP4627652B2 (en) * | 2003-10-21 | 2011-02-09 | 宇部マテリアルズ株式会社 | Magnesium oxide vapor deposition material |
| JP2007056299A (en) * | 2005-08-23 | 2007-03-08 | Kyowa Chem Ind Co Ltd | Magnesium oxide powder for vapor deposition material, and compact for vapor deposition material |
| JP5069865B2 (en) * | 2006-03-27 | 2012-11-07 | タテホ化学工業株式会社 | High purity magnesium hydroxide powder and method for producing the same |
| JP5425457B2 (en) * | 2008-12-19 | 2014-02-26 | タテホ化学工業株式会社 | Deposition material for protective film of plasma display panel |
-
2011
- 2011-03-24 JP JP2011065711A patent/JP2012201528A/en active Pending
-
2012
- 2012-02-14 CN CN2012800116524A patent/CN103415486A/en active Pending
- 2012-02-14 WO PCT/JP2012/000945 patent/WO2012127771A1/en active Application Filing
- 2012-02-16 TW TW101104998A patent/TW201238929A/en unknown
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1064147A (en) * | 1992-02-13 | 1992-09-02 | 鞍山钢铁公司 | A kind of material used as bottom of sinering furnace |
| JP2000290062A (en) * | 1999-04-05 | 2000-10-17 | Mitsubishi Materials Corp | MgO VAPOR-DEPOSITED MATERIAL AND ITS PRODUCTION |
| JP2009067603A (en) * | 2007-09-10 | 2009-04-02 | Tateho Chem Ind Co Ltd | Magnesium oxide sintered compact |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104129807A (en) * | 2014-08-05 | 2014-11-05 | 四川虹欧显示器件有限公司 | Microcrystalline material MgCaO powder, microcrystalline material as well as preparation methods and applications of MgCaO powder and microcrystalline material |
| CN106893976A (en) * | 2017-01-18 | 2017-06-27 | 东莞市佳乾新材料科技有限公司 | A kind of method for preparing MgO film as target with high-purity compact magnesia |
| CN107382283A (en) * | 2017-09-06 | 2017-11-24 | 盐城市华康电热绝缘材料厂 | The dry-pressing preparation method of magnesia ceramics |
| CN111684039A (en) * | 2018-02-16 | 2020-09-18 | 达泰豪化学工业株式会社 | Chemical heat storage material and preparation method thereof |
| JP7470246B1 (en) | 2023-11-29 | 2024-04-17 | セトラスホールディングス株式会社 | Magnesium oxide for annealing separator, its manufacturing method, and manufacturing method of grain-oriented electrical steel sheet using the same |
Also Published As
| Publication number | Publication date |
|---|---|
| WO2012127771A1 (en) | 2012-09-27 |
| JP2012201528A (en) | 2012-10-22 |
| TW201238929A (en) | 2012-10-01 |
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