CN105272226A - Preparation method of composite stabilized zirconia feed for injection molding by thermal release - Google Patents
Preparation method of composite stabilized zirconia feed for injection molding by thermal release Download PDFInfo
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- CN105272226A CN105272226A CN201510725143.3A CN201510725143A CN105272226A CN 105272226 A CN105272226 A CN 105272226A CN 201510725143 A CN201510725143 A CN 201510725143A CN 105272226 A CN105272226 A CN 105272226A
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Abstract
The inventions discloses a preparation method of composite stabilized zirconia feed for injection molding by thermal release. The preparation method includes the steps of 1 taking zirconium oxychloride and yttrium oxide as raw materials and preparing into water solution, and adding dispersants; 2 adding precipitants, and then heating for performing stirring reaction to obtain zirconium and yttrium hydroxide precipitates; 3 mixing the precipitates with deionized water for reaction; 4 placing the precipitates of step 3 into a high-temperature and high-pressure reaction kettle to undergo hydrothermal decomposition to obtain nanometer yttria stabilized zirconia powder; 5 cleaning the nanometer yttria stabilized zirconia powder; 6 performing spray drying; 7 calcinating the powder to obtain superfine stabilized zirconium powder; 8 performing ball milling, sanding and spray drying; 9 modifying, banburying, and preparing for granulating; 10 placing banbury materials into a granulator for granulating, and cutting granulates into uniform feed. The preparation method increases density and strength of ceramics, and is safer and environment-friendly.
Description
Technical field
The present invention relates to a kind of ceramic injection moulding feeding, particularly relate to the preparation method of the de-injection moulding feeding of a kind of stable composition zirconium white heat.
Background technology
Ceramic injection forming technique is a kind of high technology ceramics forming method grown up on the basis of polymer injection forming technique, it can high efficiencyly be produced in batches, and accurately can control technological process, due to controllable precise, the plastic complex-shaped ceramic component of its compact dimensions, make injection molding in ceramic molding, occupy indispensable status.
In the prior art, the injection moulding of combined oxidation zircon ceramic mainly adopts oily degreasing, then the technique of thermal debinding, the shortcoming of this technique: oil is inflammable, dangerous; Bubble oil has pollution to product; Not environmentally.Meanwhile, the organic carrier ratio of adding in compound zirconia pottery is many, occupies 13% ~ 15%, and in the process of injection moulding, inner organic carrier is not easy emptying at low temperatures, remains in density and the intensity of the organic substance influence the finished product in base substrate.
Summary of the invention
The object of the invention is to provide the preparation method of the de-injection moulding feeding of a kind of stable composition zirconium white heat, by using the method, improves density and the intensity of ceramic.
For achieving the above object, the technical solution used in the present invention is: the preparation method of the de-injection moulding feeding of a kind of stable composition zirconium white heat, the steps include:
1. with zirconium oxychloride (ZrOCl
28H
2o), yttrium oxide (Y
2o
3) for raw material is made into mixed aqueous solution 215g/L, add the dispersion agent of 1% ~ 3% simultaneously;
2. step 1. in add precipitation agent in obtained mixed aqueous solution, be then heated to 110 DEG C, constant temperature 100 hours, solution carries out stirring reaction simultaneously, obtains ultra-fine, finely dispersed zirconium hydroxide yttrium throw out;
3. by step 2. in preparation zirconium hydroxide yttrium throw out deionized water carry out allotment react;
4. by step 3. in the throw out reactor hydrothermal decomposition that is placed in High Temperature High Pressure obtain nanometer yttrium oxide stabilized zirconium oxide powder;
5. take out the nanometer yttrium oxide stabilized zirconium oxide powder of step 4. gained, clean to specific conductivity and be less than 3000us/cm;
6. spraying dry is carried out to the nanometer yttrium oxide stabilized zirconium oxide powder that 5. step is prepared;
7. the nanometer yttrium oxide stabilized zirconium oxide powder after spraying dry is calcined at 750 DEG C, obtain ultra-fine stabilised zirconia powder;
8. the ultra-fine stabilised zirconia powder after calcining is carried out ball milling, sand milling and spraying dry, obtain homodisperse superfine composite stabilised zirconia powder;
9. add organic carrier and modification is carried out to superfine composite stabilised zirconia powder: add polyethylene and SEMI-REFINED PARAFFIN WAX, oleic acid and the superfine composite zirconium powder for preparing and be placed on temperature-pressure banburying for some time in airtight Banbury mixer and, to uniform material, prepare granulation;
10. the material that banburying is good is put into granulation in tablets press, and pelletizing uniformly feeding.
In technique scheme, described step 2. in, described precipitation agent is 7.9% ammoniacal liquor (NH
3h
2o).
In technique scheme, described step 4. in, the temperature of reaction of described reactor is 103 DEG C ~ 110 DEG C.
In technique scheme, described step 9. in, described polyethylene is the Low Density Polyethylene of 10%, and described SEMI-REFINED PARAFFIN WAX is 58 degree of SEMI-REFINED PARAFFIN WAX, described in the superfine composite zirconium powder content for preparing be 90%.
In technique scheme, described step 9. in, the temperature in described Banbury mixer is 160 DEG C ~ 180 DEG C, and pressurization banburying duration is 2 hours.
In technique scheme, described step 10. in, the diameter of described feeding is 3mm, and length is 3mm ~ 4mm.
In technique scheme, described step 9. in, the content of described organic carrier is 10%.
Because technique scheme is used, the present invention compared with prior art has following advantages:
1. in the present invention, adopt content to only have the organic carrier of 10% to carry out modification to superfine composite stabilised zirconia powder, injection moulding in the injection moulding machine making the modified feeding obtained be adapted at 160 DEG C ~ 200 DEG C, then under the low temperature of 450 DEG C, thermal debinding is carried out, by the organic carrier emptying in feeding, finally under the high temperature of 1450 DEG C, sintering obtains the ceramic of high-density high-strength, with added compared with 13% ~ 15% organic carrier in the past, density and the intensity of product are stronger;
2. when feeding made in the present invention carries out injection moulding, only need Low Temperature Thermal degreasing, compared with the technique of degreasing for another example after oily degreasing in the past, product, without the need to steeping oil, can not pollute product, more environmental protection, and without the need to oil, security is stronger.
Embodiment
Below in conjunction with embodiment, the invention will be further described:
Embodiment one: the preparation method of the de-injection moulding feeding of a kind of stable composition zirconium white heat, the steps include:
1. with zirconium oxychloride (ZrOCl
28H
2o), yttrium oxide (Y
2o
3) for raw material is made into mixed aqueous solution 215g/L, add the dispersion agent of 1% ~ 3% simultaneously;
2. step 1. in add precipitation agent in obtained mixed aqueous solution, be then heated to 110 DEG C, constant temperature 100 hours, solution carries out stirring reaction simultaneously, obtains ultra-fine, finely dispersed zirconium hydroxide yttrium throw out;
3. by step 2. in preparation zirconium hydroxide yttrium throw out deionized water carry out allotment react; Described precipitation agent is 7.9% ammoniacal liquor (NH
3h
2o).
4. by step 3. in the throw out reactor hydrothermal decomposition that is placed in High Temperature High Pressure obtain nanometer yttrium oxide stabilized zirconium oxide powder, the temperature of reaction of described reactor is 103 DEG C ~ 110 DEG C.
5. take out the nanometer yttrium oxide stabilized zirconium oxide powder of step 4. gained, clean to specific conductivity and be less than 3000us/cm;
6. spraying dry is carried out to the nanometer yttrium oxide stabilized zirconium oxide powder that 5. step is prepared;
7. the nanometer yttrium oxide stabilized zirconium oxide powder after spraying dry is calcined at 750 DEG C, obtain ultra-fine stabilised zirconia powder;
8. the ultra-fine stabilised zirconia powder after calcining is carried out ball milling, sand milling and spraying dry, obtain homodisperse superfine composite stabilised zirconia powder;
9. add content be 10% organic carrier modification is carried out to superfine composite stabilised zirconia powder: the condition of modification is: the Low Density Polyethylene and 58 degree SEMI-REFINED PARAFFIN WAX, oleic acid and the content for preparing that add 10% are that 90% superfine composite zirconium powder to be placed in airtight Banbury mixer temperature-pressure banburying for some time to uniform material, preparation granulation; In this step, the temperature in Banbury mixer is 180 DEG C, and pressurization banburying duration is 2 hours.
10. the material that banburying is good is put into granulation in tablets press, and pelletizing uniformly feeding, the diameter of this feeding is 3mm, and length is 3mm ~ 4mm.
In the middle of technique in the past, adopt the organic carrier of 13% ~ 15%, organic carrier is not easily got rid of clean by idiosome degreasing under low-temperature condition of injection moulding, can cause density and the intensity of the organic substance influence the finished product remained in idiosome like this.And in the present invention, in the middle of the process manufacturing feeding, the organic carrier that only have employed 10% carries out modification to superfine composite stabilised zirconia powder, injection moulding is carried out under making the feeding finished product finally obtained be adapted at the condition of 160 DEG C ~ 200 DEG C, obtain idiosome, under the low temperature environment of 450 DEG C, carry out thermal debinding subsequently, the organic carrier in idiosome can be drained only, finally under the hot environment of 1450 DEG C, sintering obtains the ceramic of high-density, high strength.And content is that the density of the yttria-stabilized zirconia of 5% just can reach 6.08 grams/cc ~ 6.1 grams/cc.And without the need to carrying out bubble oil treatment to idiosome, can directly Low Temperature Thermal degreasing, safer, environmental protection.
Claims (7)
1. a preparation method for the de-injection moulding feeding of stable composition zirconium white heat, the steps include:
1. with zirconium oxychloride (ZrOCl
28H
2o), yttrium oxide (Y
2o
3) for raw material is made into mixed aqueous solution 215g/L, add the dispersion agent of 1% ~ 3% simultaneously;
2. step 1. in add precipitation agent in obtained mixed aqueous solution, be then heated to 110 DEG C, constant temperature 100 hours, solution carries out stirring reaction simultaneously, obtains ultra-fine, finely dispersed zirconium hydroxide yttrium throw out;
3. by step 2. in preparation zirconium hydroxide yttrium throw out deionized water carry out allotment react;
4. by step 3. in the throw out reactor hydrothermal decomposition that is placed in High Temperature High Pressure obtain nanometer yttrium oxide stabilized zirconium oxide powder;
5. take out the nanometer yttrium oxide stabilized zirconium oxide powder of step 4. gained, clean to specific conductivity and be less than 3000us/cm;
6. spraying dry is carried out to the nanometer yttrium oxide stabilized zirconium oxide powder that 5. step is prepared;
7. the nanometer yttrium oxide stabilized zirconium oxide powder after spraying dry is calcined at 750 DEG C, obtain ultra-fine stabilised zirconia powder;
8. the ultra-fine stabilised zirconia powder after calcining is carried out ball milling, sand milling and spraying dry, obtain homodisperse superfine composite stabilised zirconia powder;
9. add organic carrier and modification is carried out to superfine composite stabilised zirconia powder: add polyethylene and SEMI-REFINED PARAFFIN WAX, oleic acid and the superfine composite zirconium powder for preparing and be placed on temperature-pressure banburying for some time in airtight Banbury mixer and, to uniform material, prepare granulation;
10. the material that banburying is good is put into granulation in tablets press, and pelletizing uniformly feeding.
2. the preparation method of the de-injection moulding feeding of stable composition zirconium white according to claim 1 heat, is characterized in that: described step 2. in, described precipitation agent is 7.9% ammoniacal liquor (NH
3h
2o).
3. the preparation method of the de-injection moulding feeding of stable composition zirconium white according to claim 1 heat, is characterized in that: described step 4. in, the temperature of reaction of described reactor is 103 DEG C ~ 110 DEG C.
4. the preparation method of the de-injection moulding feeding of stable composition zirconium white heat according to claim 1, it is characterized in that: described step 9. in, described polyethylene is the Low Density Polyethylene of 10%, described SEMI-REFINED PARAFFIN WAX is 58 degree of SEMI-REFINED PARAFFIN WAX, described in the superfine composite zirconium powder content for preparing be 90%.
5. the preparation method of the de-injection moulding feeding of stable composition zirconium white according to claim 1 heat, is characterized in that: described step 9. in, the temperature in described Banbury mixer is 160 DEG C ~ 180 DEG C, and pressurization banburying duration is 2 hours.
6. the preparation method of the de-injection moulding feeding of stable composition zirconium white according to claim 1 heat, is characterized in that: described step 10. in, the diameter of described feeding is 3mm, and length is 3mm ~ 4mm.
7. the preparation method of the de-injection moulding feeding of stable composition zirconium white according to claim 1 heat, is characterized in that: described step 9. in, the content of described organic carrier is 10%.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108727015A (en) * | 2018-06-12 | 2018-11-02 | 佛山市华强协兴陶瓷有限公司 | A kind of zirconium oxide base metal-ceramic material preparation method |
| CN110002869A (en) * | 2019-05-16 | 2019-07-12 | 金业新材料科技(昆山)有限公司 | A kind of hot deoxygenated zircon ceramic injection molding feeding and preparation method thereof |
| CN110540424A (en) * | 2018-05-29 | 2019-12-06 | 山东工业陶瓷研究设计院有限公司 | Feed for zirconia ceramic injection molding and preparation method thereof |
| CN110734291A (en) * | 2019-10-31 | 2020-01-31 | 陕西博鼎快速精铸科技有限责任公司 | Processing method for ceramic mold injection molding of high-temperature-resistant polymer parts |
| CN113735579A (en) * | 2021-09-23 | 2021-12-03 | 南京金鲤新材料有限公司 | ZrO for thermal spraying2/Al2O3Method for preparing composite powder |
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| CN1374273A (en) * | 2001-03-08 | 2002-10-16 | 贵研铂业股份有限公司 | Production process of serial zirconia ceramic powder |
| CN1623905A (en) * | 2004-10-25 | 2005-06-08 | 河北鹏达新材料科技有限公司 | Method for preparing zirconium oxide micro powder |
| CN102010199A (en) * | 2010-11-19 | 2011-04-13 | 湖南正阳精密陶瓷有限公司 | Production method of zirconia ceramic bushing |
| CN103803974A (en) * | 2013-09-29 | 2014-05-21 | 雅安远创陶瓷有限责任公司 | Injection molding zirconium oxide and preparation method for same |
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2015
- 2015-10-28 CN CN201510725143.3A patent/CN105272226A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1374273A (en) * | 2001-03-08 | 2002-10-16 | 贵研铂业股份有限公司 | Production process of serial zirconia ceramic powder |
| CN1623905A (en) * | 2004-10-25 | 2005-06-08 | 河北鹏达新材料科技有限公司 | Method for preparing zirconium oxide micro powder |
| CN102010199A (en) * | 2010-11-19 | 2011-04-13 | 湖南正阳精密陶瓷有限公司 | Production method of zirconia ceramic bushing |
| CN103803974A (en) * | 2013-09-29 | 2014-05-21 | 雅安远创陶瓷有限责任公司 | Injection molding zirconium oxide and preparation method for same |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110540424A (en) * | 2018-05-29 | 2019-12-06 | 山东工业陶瓷研究设计院有限公司 | Feed for zirconia ceramic injection molding and preparation method thereof |
| CN110540424B (en) * | 2018-05-29 | 2021-12-21 | 山东工业陶瓷研究设计院有限公司 | Feed for zirconia ceramic injection molding and preparation method thereof |
| CN108727015A (en) * | 2018-06-12 | 2018-11-02 | 佛山市华强协兴陶瓷有限公司 | A kind of zirconium oxide base metal-ceramic material preparation method |
| CN110002869A (en) * | 2019-05-16 | 2019-07-12 | 金业新材料科技(昆山)有限公司 | A kind of hot deoxygenated zircon ceramic injection molding feeding and preparation method thereof |
| CN110734291A (en) * | 2019-10-31 | 2020-01-31 | 陕西博鼎快速精铸科技有限责任公司 | Processing method for ceramic mold injection molding of high-temperature-resistant polymer parts |
| CN113735579A (en) * | 2021-09-23 | 2021-12-03 | 南京金鲤新材料有限公司 | ZrO for thermal spraying2/Al2O3Method for preparing composite powder |
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