CN107129297A - A kind of preparation method of zirconium oxide composite bioceramic material - Google Patents

A kind of preparation method of zirconium oxide composite bioceramic material Download PDF

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CN107129297A
CN107129297A CN201710315538.5A CN201710315538A CN107129297A CN 107129297 A CN107129297 A CN 107129297A CN 201710315538 A CN201710315538 A CN 201710315538A CN 107129297 A CN107129297 A CN 107129297A
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zirconium oxide
zirconium
batch mixing
bioceramic material
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CN107129297B (en
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包晓刚
杨辉
陈美育
叶成清
初薛基
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SANXIANG ADVANCED MATERIALS CO Ltd
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Abstract

The present invention provides a kind of preparation method of zirconium oxide composite bioceramic material, comprises the following steps：Zirconium powder, yttrium oxide powder, beta-oxidation aluminium powder, neodymia powder and cerium oxide powder are mixed by weight 90~92: 6.0~9.0: 0.15~0.35: 0.45~0.75: 0.55~0.85, batch mixing is obtained；Added into the batch mixing after the carbon of batch mixing weight 2.0%~5.0%, put into and high melt is carried out in electric arc furnaces, after material is completely melt in stove, continue 5~30min of melting, obtain zirconium oxide liquid, blowing granulation is carried out to zirconium oxide liquid using the high hot-air of high pressure, is blown into after being cooled down in confined space and collects, then calcined, carry out breaing up grinding after cooling, then carry out temperature control in hig h-speed centrifugal spray drying, spray chamber and, at 210 DEG C~270 DEG C, obtain zirconia nanopowder bioceramic material.

Description

A kind of preparation method of zirconium oxide composite bioceramic material
Technical field
The present invention relates to bioceramic material field, specifically a kind of preparation side of zirconium oxide composite bioceramic material Method.
Background technology
With the development of modern material technology of preparing, biomaterial because possess body tissue is repaired, substitute with again Raw property, has become one of focus of current biomedical sector research.Biological hard tissue substitute material is earliest Using body bone, Animal Bone, develop into later using stainless steel and high molecule plastic, because stainless steel has dissolved, corrosion and tired The problem of labor problem, plastics existence and stability difference and low intensity.Therefore the bottleneck for causing biomaterial to develop, bioceramic goes out It is existing, the deficiency of existing alternative materials is improved, because of its many advantages, bioceramic is provided with vast potential for future development.Zirconium oxide Bioceramic belongs to bio-inert ceramic materials, good with chemical stability, the characteristics of biocompatibility is high, and with certain Mechanical strength, can be used as medical embedded product, dentistry and effective replacement of orthopedics injuries crowd's bodily tissue can be used as Material.The biomaterial made using zirconia ceramics has stable chemical property, will not produce change because of high temperature low temperature Shape, it is the most stable of product of performance in existing biomaterial, and corrosion, and zirconium oxide will not be produced because of acid-base property The organization security of ceramic making does not have any side effect.Quality requirement of certain biomedical sector for zirconium oxide bioceramic It is strict.
The content of the invention
The technical problems to be solved by the invention are：There is provided that a kind of high-compactness, stability be excellent, mechanical strength is good The preparation method of zirconium oxide composite bioceramic material.
In order to solve the above-mentioned technical problem, the technical solution adopted by the present invention is：A kind of zirconium oxide composite boilogical ceramic material The preparation method of material, comprises the following steps：
Step 1, by Zirconium powder, yttrium oxide powder, beta oxidation aluminium powder, neodymia powder and cerium oxide powder by weight 90~92: 6.0~9.0: 0.15~0.35: 0.45~0.75: 0.55~0.85 is mixed, and obtains batch mixing；
Step 2, add after the carbon of batch mixing weight 2.0%~5.0% into the batch mixing, carried out in input electric arc furnaces high Warm melting, after material is completely melt in stove, continues 5~30min of melting, obtains zirconium oxide liquid；
Step 3, step 2 gained zirconium oxide liquid is toppled over and come out of the stove, using 1400 DEG C, 25~more than 35MPa high pressure hyperpyrexia Air carries out blowing granulation to zirconium oxide liquid, is blown into after being cooled down in confined space and collects；
Step 4, step 3 gains are placed in 1000 DEG C~1200 DEG C roller kilns calcining 120min~300min, cooling After collect；
Step 5, step 4 gains are delivered to superfine sand mill carry out breaing up grinding, control ground slurry quality percentage dense Degree 25%~45%, milling time 20min~90min；
Step 6, by step 5 gains feeding spray dryer carry out hig h-speed centrifugal spray drying, spray indoor temperature control System obtains zirconia nanopowder bioceramic material at 210 DEG C~270 DEG C.
The beneficial effects of the present invention are：Prior art is different from, zirconia nanopowder biology pottery made from the inventive method Ceramic material chemical constituent is merged with liquid, and uniformity and stability are good, and it is small to vary with temperature bulk effect, passes through high pressure-temperature oxygen Gas blowout, which is blown, can directly be blown into nano-powder, it is to avoid force crushing grinding process to introduce the impurity such as machinery iron.Make after product Detection bulk density can reach 5.60g/cm3~5.80g/cm3, the porosity is low, with the existing chemical method product phase of in the market Than, high purity nanometer powders can be equally prepared, meanwhile, production procedure is short, and cost is low, and production process environmental pollution is small.Yin Qigao's Bulk density and few porosity, downstream product mechanical strength and service life can be effectively improved for downstream product.To be electricity Make very big contribution in molten method production bioceramic material field.
Embodiment
To describe technology contents, the objects and the effects of the present invention in detail, it is explained below in conjunction with embodiment.
The design of most critical of the present invention is：Realize that each component fully melts under high-temperature liquid state by electro-smelting first Close, booster tension carries out depth melting in order to which the volatile matter such as charcoal element impurity is discharged, and is compressed and sprayed simultaneously using 25~35MPa The high hot-air of high pressure of journey electrical heating to more than 1400 DEG C carries out blowing granulation slurries are blown into ultra-fine receive to zirconium oxide liquid The other powder of meter level, then 1000 DEG C~1200 DEG C roller kilns progress dynamic calcining 120min~300min are placed in, to discharge residual Volatile matter impurity.With superfine sand mill break up and be sent directly into spray dryer after grinding and be dried, be for the powder that will reunite Body is broken up out, and to recover product primary particle size, increases product specific surface area.
The present invention provides a kind of preparation method of zirconium oxide composite bioceramic material, comprises the following steps：
Step 1, by Zirconium powder, yttrium oxide powder, beta oxidation aluminium powder, neodymia powder and cerium oxide powder by weight 90~92: 6.0~9.0: 0.15~0.35: 0.45~0.75: 0.55~0.85 is mixed, and obtains batch mixing；
Step 2, add after the carbon of batch mixing weight 2.0%~5.0% into the batch mixing, carried out in input electric arc furnaces high Warm melting, after material is completely melt in stove, continues 5~30min of melting, obtains zirconium oxide liquid；
Step 3, step 2 gained zirconium oxide liquid is toppled over and come out of the stove, using 1400 DEG C, 25~more than 35MPa high pressure hyperpyrexia Air carries out blowing granulation to zirconium oxide liquid, is blown into after being cooled down in confined space and collects；
Step 4, step 3 gains are placed in 1000 DEG C~1200 DEG C roller kilns calcining 120min~300min, cooling After collect；
Step 5, step 4 gains are delivered to superfine sand mill carry out breaing up grinding, control ground slurry quality percentage dense Degree 25%~45%, milling time 20min~90min；
Step 6, by step 5 gains feeding spray dryer carry out hig h-speed centrifugal spray drying, spray indoor temperature control System obtains zirconia nanopowder bioceramic material at 210 DEG C~270 DEG C.
Further, the raw material Zirconium powder, yttrium oxide powder, beta oxidation aluminium powder, neodymia powder and cerium oxide Powder grade is >=99.999%.
Further, in step 1, mixing is to force to carry out in blender, and incorporation time is 30min~150min.
Further, in step 2, arc melting voltage is controlled in 180V~260V, and electric current is in 6KA-15KA.
It was found from foregoing description, zirconia nanopowder bioceramic material chemical constituent is melted with liquid made from the inventive method Close, uniformity and stability is good, it is small to vary with temperature bulk effect, can be directly blown into and received by high pressure-temperature blowing oxygen Ground rice body, it is to avoid force crushing grinding process to introduce the impurity such as machinery iron.Make and detect that bulk density can reach after product 5.60g/cm3~5.80g/cm3, the porosity is low, compared with the existing chemical method product of in the market, can equally prepare high-purity nm Powder, meanwhile, production procedure is short, and cost is low, and production process environmental pollution is small.Yin Qigao bulk density and few porosity, Downstream product mechanical strength and service life can be effectively improved for downstream product.To be electric smelting method production bioceramic material neck Make very big contribution in domain.
Embodiment 1
1. by the Zirconium powder of purity 99.999%, yttrium oxide powder, beta oxidation aluminium powder, neodymia powder and cerium oxide powder Body is 91.32 by mass percentage:7.95:0.15:0.45:0.53 carries out dispensing；
2. forcing to carry out mixing 35min in blender；
3. after above raw material is well mixed, 2.15% high purity graphite carbon, input cleaning in advance are incorporated in mass ratio High melt is carried out in good electric arc furnaces.Control arc melting voltage 190V, melting electric current 8.6KA；
4. after being completely melt in stove, the melting voltage of control lifting electric arc furnaces is to 205V, then carries out melting 9min, to fill Divide stirring fusion, while discharging charcoal element and volatile matter；
Come out of the stove 5. toppling over, the high hot-air pair of high pressure for spraying process electrical heating to 1420 DEG C simultaneously is compressed using 29.8MPa Zirconium oxide liquid carries out blowing granulation, is blown into sufficiently large confined chamber, is collected after blowout product natural cooling to be painted；
6. the said goods are placed in 1090 DEG C of roller kilns and carry out dynamic calcining 145min again, miscellaneous to discharge residual volatile matter Matter；
7. calcined product natural cooling is collected, deliver to superfine sand mill and carry out breaing up grinding, control stock quality percentage Concentration 36%, milling time 25min；
8. ground slurry feeding Highspeedcentrifugingandsprayingdrier is dried, spray chamber's temperature is controlled at 247 DEG C；
9. collecting spray drying powder, required zirconia nanopowder bioceramic powder material is finally given.
Embodiment 2
A kind of preparation method of zirconium oxide composite bioceramic material, comprises the following steps：
Step 1, by Zirconium powder, yttrium oxide powder, beta oxidation aluminium powder, neodymia powder and cerium oxide powder by weight 90: 6.0: 0.15: 0.45: 0.55 with forcing blender to mix, and incorporation time is 30min, obtains batch mixing；
Step 2, add after the carbon of batch mixing weight 2.0% into the batch mixing, high melt carried out in input electric arc furnaces, After material is completely melt in stove, continues melting 5min, obtain zirconium oxide liquid, wherein, the control of arc melting voltage is in 180V, electricity Stream is in 6KA；
Step 3, step 2 gained zirconium oxide liquid is toppled over and come out of the stove, using the high hot-air of the high pressure of 1400 DEG C, 35MPa to oxygen Change zirconium liquid and carry out blowing granulation, be blown into after being cooled down in confined space and collect；
Step 4, step 3 gains are placed in 1000 DEG C of roller kilns calcining 120min, collected after cooling；
Step 5, step 4 gains are delivered to superfine sand mill carry out breaing up grinding, control ground slurry quality percentage dense Degree 25%, milling time 20min；
Step 6, by step 5 gains feeding spray dryer carry out hig h-speed centrifugal spray drying, spray indoor temperature control System obtains zirconia nanopowder bioceramic material at 210 DEG C.
Embodiment 3
A kind of preparation method of zirconium oxide composite bioceramic material, comprises the following steps：
Step 1, by Zirconium powder, yttrium oxide powder, beta oxidation aluminium powder, neodymia powder and cerium oxide powder by weight 92: 9.0: 0.35: 0.75: 0.85 with forcing blender to mix, and incorporation time is 150min, obtains batch mixing；
Step 2, add after the carbon of batch mixing weight 5.0% into the batch mixing, high melt carried out in input electric arc furnaces, After material is completely melt in stove, continues melting 30min, obtain zirconium oxide liquid, wherein, arc melting voltage is controlled in 260V, Electric current is in 15KA；
Step 3, step 2 gained zirconium oxide liquid is toppled over and come out of the stove, using the high hot-air of the high pressure of 1500 DEG C, 35MPa to oxygen Change zirconium liquid and carry out blowing granulation, be blown into after being cooled down in confined space and collect；
Step 4, step 3 gains are placed in 1200 DEG C of roller kilns calcining 300min, collected after cooling；
Step 5, step 4 gains are delivered to superfine sand mill carry out breaing up grinding, control ground slurry quality percentage dense Degree 45%, milling time 90min；
Step 6, by step 5 gains feeding spray dryer carry out hig h-speed centrifugal spray drying, spray indoor temperature control System obtains zirconia nanopowder bioceramic material at 270 DEG C.
Embodiment 4
A kind of preparation method of zirconium oxide composite bioceramic material, comprises the following steps：
Step 1, by Zirconium powder, yttrium oxide powder, beta oxidation aluminium powder, neodymia powder and cerium oxide powder by weight 91: 7.5: 0.25: 0.55: 0.75 with forcing blender to mix, and incorporation time is 30min~150min, obtains batch mixing；
Step 2, add after the carbon of batch mixing weight 3.5% into the batch mixing, high melt carried out in input electric arc furnaces, After material is completely melt in stove, continues melting 17.5min, obtain zirconium oxide liquid, wherein, the control of arc melting voltage exists 220V, electric current is in 10KA；
Step 3, step 2 gained zirconium oxide liquid is toppled over and come out of the stove, using the high hot-air of the high pressure of 1800 DEG C, 30MPa to oxygen Change zirconium liquid and carry out blowing granulation, be blown into after being cooled down in confined space and collect；
Step 4, step 3 gains are placed in 1100 DEG C of roller kilns calcining 210min, collected after cooling；
Step 5, step 4 gains are delivered to superfine sand mill carry out breaing up grinding, control ground slurry quality percentage dense Degree 35%, milling time 55min；
Step 6, by step 5 gains feeding spray dryer carry out hig h-speed centrifugal spray drying, spray indoor temperature control System obtains zirconia nanopowder bioceramic material at 240 DEG C.
In summary, zirconia nanopowder bioceramic material chemical constituent is merged with liquid made from the inventive method, Even property and stability are good, and it is small to vary with temperature bulk effect, and nano powder can be directly blown into by high pressure-temperature blowing oxygen Body, it is to avoid force crushing grinding process to introduce the impurity such as machinery iron.Make and detect that bulk density can reach 5.60g/ after product cm3~5.80g/cm3, the porosity is low, compared with the existing chemical method product of in the market, can equally prepare high purity nanometer powders, together When, production procedure is short, and cost is low, and production process environmental pollution is small.Yin Qigao bulk density and few porosity, for downstream Product can effectively improve downstream product mechanical strength and service life.Pole will be made for electric smelting method production bioceramic material field Big contribution.
Embodiments of the invention are the foregoing is only, are not intended to limit the scope of the invention, it is every to utilize this hair The equivalents that bright description is made, or the technical field of correlation is directly or indirectly used in, similarly it is included in this hair In bright scope of patent protection.

Claims (4)

1. a kind of preparation method of zirconium oxide composite bioceramic material, it is characterised in that：Comprise the following steps：
Step 1, by Zirconium powder, yttrium oxide powder, beta oxidation aluminium powder, neodymia powder and cerium oxide powder by weight 90~ 92: 6.0~9.0: 0.15~0.35: 0.45~0.75: 0.55~0.85 is mixed, and obtains batch mixing；
Step 2, add after the carbon of batch mixing weight 2.0%~5.0% into the batch mixing, high temperature melting is carried out in input electric arc furnaces Refining, after material is completely melt in stove, continues 5~30min of melting, obtains zirconium oxide liquid；
Step 3, step 2 gained zirconium oxide liquid is toppled over and come out of the stove, using the high hot-air of the high pressure of 1400 DEG C, 25~more than 35MPa Blowing granulation is carried out to zirconium oxide liquid, is blown into after being cooled down in confined space and collects；
Step 4, step 3 gains are placed in 1000 DEG C~1200 DEG C roller kilns calcining 120min~300min, received after cooling Collection；
Step 5, step 4 gains are delivered to superfine sand mill carry out breaing up grinding, control ground slurry mass percentage concentration 25%~45%, milling time 20min~90min；
Step 6, step 5 gains feeding spray dryer is subjected to hig h-speed centrifugal spray drying, temperature control exists in spray chamber 210 DEG C~270 DEG C, obtain zirconia nanopowder bioceramic material.
2. the preparation method of zirconium oxide composite bioceramic material according to claim 1, it is characterised in that：The former material Expect that Zirconium powder, yttrium oxide powder, beta oxidation aluminium powder, neodymia powder and cerium oxide powder grade are >=99.999%.
3. the preparation method of zirconium oxide composite bioceramic material according to claim 1, it is characterised in that：In step 1, Mixing is to force to carry out in blender, and incorporation time is 30min~150min.
4. the preparation method of zirconium oxide composite bioceramic material according to claim 1, it is characterised in that：In step 2, Arc melting voltage is controlled in 180V~260V, and electric current is in 6KA-15KA.
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