CN1093105C - Kiln aparatus and method for preparing zirconium oxide used in electronic industry - Google Patents

Abstract

The present invention relates to zirconium oxide kiln furniture for electronic industry and a manufacturing method thereof. Electric melting zirconium oxide raw materials are used as basal bodies, calcium oxide and yttrium oxide used as stabilizing agents are added, and the mixture is calcined by an electric arc furnace; then after ball milling, vibration milling, dry pressing or slip casting and drying are carried out, the mixture is calcined at 1550 to 1650 DEG C to obtain the zirconium oxide kiln furniture of the present invention. Because the added stabilizing agents are different, the present invention has two different products; when calcium oxide is used as stabilizing agents, the kiln furniture comprises the chemical compositions: 90 to 95% of ZrO2 and 3.5 to 4.5% of CaO; when yttrium oxide is used as stabilizing agents, the kiln furniture comprises the chemical compositions: 88 to 93% of ZrO2 and 6 to 10% of Y2O3. In addition, the two products respectively comprise the compositions: 0.1 to 0.4% of TiO2, 0.4 to 1.2% of Al2O3, 0.4 to 1.2% of SiO2 and at most 0.2 of Fe2O3.

Description

Zirconium oxide used in electronic industry kiln furnitures and manufacture method thereof

The present invention relates to a kind of zirconium white kiln furnitures and manufacture method thereof, more particularly, the invention relates to the two kinds of chemical constitutions of zirconium white kiln furnitures and the technology of manufacture method, belong to the special ceramics technical field.

Mn-Zn system and Ni-Zn that the senior kiln furnitures of zirconium oxide used in electronic industry are mainly used in chip ceramic capacitor, wafer capacitance device, mesohigh ceramic condenser and the magneticsubstance class of electronic ceramics class are fields such as soft magnetic materials, and as the backing plate of above these materials in sintering process.

The conventional fabrication processes that is used for the Mn-Zn system of chip ceramic capacitor, wafer capacitance device, mesohigh ceramic condenser and magneticsubstance of electronic ceramics class and Ni-Zn and is the backing plate that soft magnetic materials burns till has following several:

1, adopt the zirconium white powder as insulating powder be sprinkling upon burn material around;

2, adopt electric-melting zirconia without calcium oxide or stabilized with yttrium oxide as raw material, dry-pressing formed through ball mill pulverizing, batching, adding tackiness agent, in air, burn till in 1600 ℃, make the zirconium white kiln furnitures.

The shortcoming of above-mentioned manufacture method is:

1, adopt the zirconium white powder to be difficult for spreading even as insulating powder, and, easily the burning material caused scuffing because powder has certain particle, so influence burn the quality of product.

2, adopt the zirconium white kiln furnitures of making as raw material without the electric-melting zirconia of calcium oxide or stabilized with yttrium oxide, because the inherent characteristic of zirconium white own, in use can be with about 7% volume change, density and void content can not be controlled effectively, very easily efflorescence of life-time service, cracking, work-ing life, reliability was relatively poor less than 30 days, brought a lot of inconvenience to the user.

The composition and the manufacture method that the purpose of this invention is to provide a kind of zirconium white kiln furnitures.It is raw material that the prepared zirconium white kiln furnitures of this method adopt the capacitive oxidation zirconium of calcium oxide and stabilized with yttrium oxide, and not only density and void content can be controlled effectively, and adopts mechanize production, and production efficiency improves greatly, helps large-scale production.

The composition of zirconium white kiln furnitures of the present invention is because of added stablizer difference, and two kinds of different chemical constitutions are arranged.

When 1, being stablizer with the calcium oxide, the chemical constitution of kiln furnitures is ZrO ₂90-95%, TiO ₂0.1-0.4%, Al ₂O ₃0.4-1.2%, SiO ₂0.4-1.2%, CaO 3.5-4.5%, Fe ₂O ₃＜0.2%;

When 2, being stablizer with the yttrium oxide, the chemical constitution of kiln furnitures is ZrO ₂88-93%, TiO ₂0.1-0.4%, Al ₂O ₃0.4-1.2%, SiO ₂0.4-1.2%, Y ₂O ₃6-10%, Fe ₂O ₃＜0.2%.

The manufacture method of zirconium white kiln furnitures of the present invention:

1, being is major ingredient with the zirconium white, ZrO ₂Content 94-98% is as TiO ₂, AL ₂O ₃, SiO ₂, Fe ₂O ₃, reaching other a small amount of innoxious substance and volatile matter total amount is 2-6%.

With calcium oxide or yttrium oxide is stablizer, and electric smelting in electric arc blows out the hollow ball of φ 2-10mm with air compressor machine, and hollow ball is carried out ball milling, and powder is made in vibration, and the powder fineness is average particle size≤0.2mm, ZrO in this material ₂Cube be 70-90% mutually; Add suitable amount of adhesive in the powder, make the semi-drying mixture, dry-pressing formed after granulation, place 80-120 ℃ of drying room to dry dry-pressing formed base substrate; To dry base substrate so that whenever folded 16-36 sheet is superimposed neat, lie on the load bearing board,, be incubated 0.5-2.5 hour at 1550 ℃ of-1650 ℃ of following sintering.Above-mentioned load bearing board is made by corundum-mullite, and its corundum content is not less than 75%.

For selecting for use of capacitive oxidation zirconium raw material, should be able to satisfy the requirement of above-mentioned two kinds of kiln furnitures compositions.

The invention will be further described below in conjunction with embodiment.

Table 1-3 provides two groups of embodiment of the present invention totally 6 samples compositions.

First group of embodiment (sample 1-3) has the characteristic of the good anti-glass attack of high temperature resistant resistance to chemical attack; Second group of embodiment (sample 4-6) has the characteristic of fabulous high temperature resistant resistance to chemical attack.

Table 1

Sample main component (weight %) numbering ZrO ₂TiO ₂CaO SiO ₂Al ₂O ₃Fe ₂O ₃OTHER1 92.9 0.3 4.4 0.8 1.2 0.2 0.22 93.6 0.3 4.1 0.8 0.8 0.2 0.23 94.4 0.2 3.8 0.6 0.6 0.2 0.2 table 2 sample main components (weight %) numbering ZrO ₂TiO ₂Y ₂O ₆SiO ₂Al ₂O ₃Fe ₂O ₃OTHER1 90.7 0.2 8.0 0.5 0.4 0.1 0.12 91.4 0.2 7.2 0.5 0.5 0.1 0.13 92.2 0.2 6.3 0.5 0.6 0.1 0.1

The main raw material of said products adopts the electric smelting manufactured.Powder average grain is about 0.2 millimeter by above-mentioned prescription mixes with distilled water in the nylon jar, adds tackiness agent, stirs then 10 minutes, make the leather hard mixture, dry-pressing formed, thickness is the 5-10 millimeter, put into baking oven and carry out drying, drying temperature is 80-120 ℃; The whenever folded 16-36 sheet of above-mentioned disk base substrate is superimposed neat, lie against on the load bearing board, sample 1-3 is incubated 1 hour at 1600 ℃ of following sintering; Sample 4-6 is incubated 0.5-2.5 hour at 1580 ℃ of following sintering.

The performance of above-mentioned each sample is shown in the table 3.Table 3 sample density void content numbering (g/cm3) (%) 1 3.6 252 4.0 223 4.4 194 4.1 285 4.0 266 4.1 25

The present invention compared with prior art has the following advantages:

1, the zirconia kiln furnitures adopt the electric-melting zirconia of calcium oxide or stabilized with yttrium oxide, and material property is steady Fixed, the reliability excellence.

2, the zirconia kiln furnitures can be made density, the porosity at product, density and the pore of certain limit Rate can be controlled effectively, is conducive to the instructions for use of different electronic ceramics.

3, having good stability of zirconia kiln furnitures, and its high temperature resistant resistance to chemical attack resistance to glass attack Excellent performance, thus can guarantee not pollute the electronic ceramics product, significantly improve the finished product of electronic ceramics product Rate and qualification rate.

4, the zirconia kiln furnitures are when finish service life, can reclaim and through being reprocessed into new product, Re-use, avoided environmental pollution.

Claims (6)

1, a kind of zirconium oxide used in electronic industry kiln furnitures, when it is characterized in that described product is stablizer with the calcium oxide, the chemical constitution of kiln furnitures is ZrO ₂90-95%, TiO ₂0.1-0.4%, Al ₂O ₃0.4-1.2%, SiO ₂0.4-1.2%, CaO3.5-4.5%, Fe ₂O ₃＜0.2%.

2, a kind of manufacture method of zirconium oxide used in electronic industry kiln furnitures as claimed in claim 1 is characterized in that:

1.1 be to be major ingredient with the zirconium white, ZrO ₂Content 94-98% also has TiO ₂, Al ₂O ₃, SiO ₂, Fe ₂O ₃Reaching other a small amount of innoxious substance and volatile matter total amount is 2-6%;

1.2 above-mentioned electric-melting zirconia raw material calcium oxide is a stablizer, electric smelting in electric arc blows out the hollow ball of φ 2-10mm with air compressor machine;

1.3 above-mentioned hollow ball is carried out ball milling, and powder is made in vibration, the powder fineness is average particle size≤0.2mm, ZrO ₂Cube be 70-90% mutually;

1.4 will add tackiness agent in the powder, make the semi-drying mixture, dry-pressing formed after granulation, place 80-120 ℃ of drying room to dry dry-pressing formed base substrate;

1.5 above-mentioned oven dry base substrate so that whenever folded 16-36 sheet is superimposed neat, is lain on the load bearing board,, is incubated 0.5-2.5 hour at 1550 ℃ of-1650 ℃ of following sintering.

3, the manufacture method of zirconium oxide used in electronic industry kiln furnitures according to claim 2 is characterized in that: described load bearing board is made by corundum-mullite, and its corundum content is not less than 75%.

4, a kind of zirconium oxide used in electronic industry kiln furnitures, when it is characterized in that described product is stablizer with the yttrium oxide, the chemical constitution of kiln furnitures is ZrO ₂88-93%, TiO ₂0.1-0.4%, Al ₂O ₃0.4-1.2%, SiO ₂0.4-1.2%, Y ₂O ₂6-10%, Fe ₂O ₃＜0.2%.

5, a kind of manufacture method of zirconium oxide used in electronic industry kiln furnitures as claimed in claim 4 is characterized in that:

1.1 be to be major ingredient with the zirconium white, ZrO ₂Content 94-98% also has TiO ₂, Al ₂O ₃, SiO ₂, Fe ₂O ₃Reaching other a small amount of innoxious substance and volatile matter total amount is 2-6%;

1.2 above-mentioned electric-melting zirconia raw material yttrium oxide is a stablizer, electric smelting in electric arc blows out the hollow ball of φ 2-10mm with air compressor machine;

1.3 above-mentioned hollow ball is carried out ball milling, and powder is made in vibration, the powder fineness is average particle size≤0.2mm, ZrO ₂Cube be 70-90% mutually;

1.4 will add tackiness agent in the powder, make the semi-drying mixture, dry-pressing formed after granulation, place 80-120 ℃ of drying room to dry dry-pressing formed base substrate;

1.5 above-mentioned oven dry base substrate so that whenever folded 16-36 sheet is superimposed neat, is lain on the load bearing board,, is incubated 0.5-2.5 hour at 1550 ℃ of-1650 ℃ of following sintering.

6, the manufacture method of zirconium oxide used in electronic industry kiln furnitures according to claim 5 is characterized in that: described load bearing board is made by corundum-mullite, and its corundum content is not less than 75%.