CN102432274A

CN102432274A - Production process for alumina ceramic target

Info

Publication number: CN102432274A
Application number: CN2011102842513A
Authority: CN
Inventors: 陈海军
Original assignee: Individual
Current assignee: Individual
Priority date: 2011-09-18
Filing date: 2011-09-18
Publication date: 2012-05-02
Anticipated expiration: 2031-09-18
Also published as: CN102432274B

Abstract

The invention discloses a production process for alumina ceramic targets. The process comprises the following steps: 1) placing high purity aluminum hydroxide into a crucible for pyrolysis to produce high purity alumina particles, then producing alumina particulates and finally preparing alumina particles with a particle size of 35 to 50 mu m; 2) preparing alumina spheres with a size of 2 to 4 mm; 3) pressing alumina spheres into targets with a variety of shapes at a temperature of 25 to 100 DEG C under a pressure of 100 MPA, wherein, during pressing, the temperature of the alumina spheres is maintained at 25 to 100 DEG C, and a forming pressure is maintained at 100 MPA; 4) carrying out high temperature sintering on the press formed targets three times; 5) packaging obtained products. The beneficial effects of the invention are as follows: the alumina targets produced by using the process have the characteristics of high purity, great density, good toughness, a slightly shrunken body and high yield of good products.

Description

A kind of production technique of aluminium sesquioxide ceramic target

Technical field

The present invention relates to a kind of production technique of ceramic target, particularly a kind of production technique of aluminium sesquioxide ceramic target.

Background technology

Existing in the market aluminium sesquioxide target generally is a crystalline material; Also there is simultaneously a spot of aluminium sesquioxide ceramic target; This type of aluminium sesquioxide ceramic target adopts the powder body material direct forming, thereby exists the shortcoming that product density is low, fragility is big, sintering temperature is high, sintering process is shunk greatly, body is yielding and good article rate is low.

Summary of the invention

The problem that the present invention will solve is: a kind of production technique of aluminium sesquioxide ceramic target is provided, and the aluminium sesquioxide target that is come out by this explained hereafter has the advantages that product density is big, the body shrinking percentage is little, body is not yielding and the product yield is high.

In order to solve the problems of the technologies described above, the production technique of aluminium sesquioxide ceramic target of the present invention may further comprise the steps:

1) high purity aluminium hydroxide is put into crucible, with sintering oven the high purity aluminium hydroxide in the crucible is heated to 1200 ℃ and carries out pyrolytic decomposition, decompose generation high purity aluminium sesquioxide particle; Particle size is sent to feed chamber with the aluminium sesquioxide particle that generates through the follower arm of micronizer mill then at the 35-45 micron, and the aluminium sesquioxide particle falls into crushiing chamber under action of gravity; Being provided with the high pressure admission nozzle of arranging in opposite directions around the crushiing chamber, is the pressurized air of 0.8-1Mpa through purification and exsiccant pressure, penetrates from nozzle; Form hypersonic air flow, the aluminium sesquioxide particle is pulverized in moment in high velocity air intersection point Central Collisions; Generate the aluminium sesquioxide particulate, particle size is put into the aluminium sesquioxide particulate in the spray granulating and drying machine below 0.5 micron again; Start the spray granulating and drying machine; The aluminium sesquioxide particulate contact through the high-temperature hot air of spraying gun atomizing back ejection droplet with 300 ℃, and moisture is evaporated, the solid fines that wets further drying and drop down onto the atomizing granulation zone in dropping process; Contact simultaneously with the aluminium sesquioxide powder that in fluidized-bed, flies upward come-up with hot gas flow; The aluminium sesquioxide particle of formation 35-50 micron gets into the fluidized-bed at the bottom of the tower, and fluidized-bed temperature is 200 ℃, and the aluminium sesquioxide particle that gets into fluidized-bed was at fluidised bed drying 30-45 minute; Aluminium sesquioxide particulate moisture is discharged, make aluminium sesquioxide particle water cut be lower than 1%;

The aluminium sesquioxide particulate of the 35-50 micron that 2) step 1 is generated is put in the spray granulating and drying machine; Under the running of spray granulating and drying machine, aluminium sesquioxide particle ejection droplet after the spraying gun atomizing contacts with high-temperature hot air, and moisture is evaporated; Wet solid fines is further dry and drop down onto the atomizing granulation zone in dropping process; Contact with the aluminium sesquioxide powder that in fluidized-bed, flies upward come-up with hot gas flow simultaneously, the aluminium sesquioxide ball of formation 2-4mm is then 300 ℃-400 ℃ sintering temperature 3 hours; Get rid of the steam of aluminium sesquioxide ball the inside, processing purity is the aluminium sesquioxide spheroid of 99.99-99.999%;

3) at 25 ℃--under 100 ℃, the environment of 100MPA, the aluminium sesquioxide spheroid that step 2 is generated is pressed into the ceramic target of all kinds of bodies; Keeping aluminium sesquioxide spheroid temperature during compacted products is 25 ℃--100 ℃, compacting pressure is 100MPA;

4) ceramic target to compression moulding carries out high temperature sintering three times, and first sintering adopts 1200 ℃ of normal pressure pre-burnings, is incubated 2-4 hour; Sintering adopts temperature at 1300-1600 ℃ for the second time, and vacuum tightness reaches 0.0025PA. insulation 3-6 hour, uses nitrogen as shielding gas. and the insulation back adopts the mode of naturally cooling to accomplish sintering for the second time; Sintering is a de-stress sintering under normal pressure for the third time, is sintered to 1200 ℃ of top temperatures by normal temperature, under this temperature, needs insulation 4 hours, naturally cools to then below 100 ℃;

5) product is packed.

The beneficial effect that the present invention obtains is: by the aluminium sesquioxide ceramic target that cover process is produced, have that purity height, density are big, good toughness, body shrink characteristics little and that the product non-defective unit is high.

Embodiment

When specifically producing the aluminium sesquioxide target, adopt following steps:

The first step is put into crucible with the 500g high purity aluminium hydroxide, with sintering oven the high purity aluminium hydroxide in the crucible is heated to 1200 ℃ and carries out pyrolytic decomposition; Decompose generation high purity aluminium sesquioxide particle, particle size is sent to feed chamber with the aluminium sesquioxide particle that generates through the follower arm of micronizer mill then at the 35-45 micron; The aluminium sesquioxide particle falls into crushiing chamber under action of gravity, is provided with the high pressure admission nozzle of arranging in opposite directions around the crushiing chamber, is the pressurized air of 0.8-1Mpa through purification and exsiccant pressure; Penetrate from nozzle, form hypersonic air flow, the aluminium sesquioxide particle is in high velocity air intersection point Central Collisions; Pulverized in moment, generate the aluminium sesquioxide particulate, particle size is below 0.5 micron; The aluminium sesquioxide particulate is put in the spray granulating and drying machine again, started the spray granulating and drying machine, the aluminium sesquioxide particulate sprays droplet and contacts with 300 ℃ high-temperature hot air through spraying gun atomizing back; Moisture is evaporated; Wet solid fines is further dry and drop down onto the atomizing granulation zone in dropping process, contact with the aluminium sesquioxide powder that in fluidized-bed, flies upward come-up with hot gas flow simultaneously, forms the fluidized-bed at the bottom of the aluminium sesquioxide particle entering tower of 35-50 micron; Fluidized-bed temperature is 200 ℃; The aluminium sesquioxide particle that gets into fluidized-bed was discharged aluminium sesquioxide particulate moisture at fluidised bed drying 30-45 minute, made aluminium sesquioxide particle water cut be lower than 1%;

Second step; The aluminium sesquioxide particulate of the 35-50 micron that step 1 is generated is put in the spray granulating and drying machine; Under the running of spray granulating and drying machine, aluminium sesquioxide particle ejection droplet after the spraying gun atomizing contacts with high-temperature hot air, and moisture is evaporated; Wet solid fines is further dry and drop down onto the atomizing granulation zone in dropping process; Contact with the aluminium sesquioxide powder that in fluidized-bed, flies upward come-up with hot gas flow simultaneously, the aluminium sesquioxide ball of formation 2-4mm is then 300 ℃-400 ℃ sintering temperature 3 hours; Get rid of the steam of aluminium sesquioxide ball the inside, processing purity is the aluminium sesquioxide spheroid 498.2g of 99.99-99.999%;

The 3rd step, at 25 ℃--under 100 ℃, the environment of 100MPA, the aluminium sesquioxide spheroid that step 2 is generated is pressed into the ceramic target of all kinds of bodies; Keeping aluminium sesquioxide spheroid temperature during compacted products is 25 ℃--100 ℃, compacting pressure is 100MPA;

The 4th step, the ceramic target of compression moulding is carried out high temperature sintering three times, first sintering adopts 1200 ℃ of normal pressure pre-burnings, is incubated 2-4 hour; Sintering adopts temperature at 1300-1600 ℃ for the second time, and vacuum tightness reaches 0.0025PA. insulation 3-6 hour, uses nitrogen as shielding gas. and the insulation back adopts the mode of naturally cooling to accomplish sintering for the second time; Sintering is a de-stress sintering under normal pressure for the third time, is sintered to 1200 ℃ of top temperatures by normal temperature, under this temperature, needs insulation 4 hours, naturally cools to then below 100 ℃, obtains the aluminium sesquioxide ceramic target 497.6g that sinters at last;

In the 5th step, product is packed.

Patent of the present invention adopts the high purity aluminium oxide powder as the basis; Powder body material is carried out secondary granulation; Generate the aluminium sesquioxide spheroid of 2-4 millimeter, again through constant temperature, constant voltage, the forming technology when permanent is produced all kinds of body ceramic targets; Thereby the aluminium sesquioxide ceramic target purity of being produced by patent of the present invention is high, can reach 99.99-99.999%; Density is big, and the effect of inner spherical grain disperses its stress behind the presswork, and toughness of products is good; Repeatedly granulation and high-pressure forming make product have greater density, in sintering process, reduce by 200 ℃ of sintering temperatures, thereby cut down the consumption of energy, and the product density behind the completion sintering changes little, and body shrinks little, and the good article rate of sintering process can reach 99.5%.

Claims

1. the production technique of an aluminium sesquioxide ceramic target is characterized in that may further comprise the steps:

3) at 25 ℃--under 100 ℃, the environment of 100MPA, the aluminium sesquioxide spheroid that step 2 is generated is pressed into the target of all kinds of bodies; Keeping aluminium sesquioxide spheroid temperature during compacted products is 25 ℃--100 ℃, compacting pressure is 100MPA;

4) target to compression moulding carries out high temperature sintering three times, and first sintering adopts 1200 ℃ of normal pressure pre-burnings, is incubated 2-4 hour; Sintering adopts temperature at 1300-1600 ℃ for the second time, and vacuum tightness reaches 0.0025PA. insulation 3-6 hour, uses nitrogen as shielding gas. and the insulation back adopts the mode of naturally cooling to accomplish sintering for the second time; Sintering is a de-stress sintering under normal pressure for the third time, is sintered to 1200 ℃ of top temperatures by normal temperature, under this temperature, needs insulation 4 hours, naturally cools to then below 100 ℃;

5) product is packed.