CN101429018A - Freezing molding method for neodymium doped yttrium aluminum garnet transparent laser ceramic - Google Patents
Freezing molding method for neodymium doped yttrium aluminum garnet transparent laser ceramic Download PDFInfo
- Publication number
- CN101429018A CN101429018A CNA2008102379708A CN200810237970A CN101429018A CN 101429018 A CN101429018 A CN 101429018A CN A2008102379708 A CNA2008102379708 A CN A2008102379708A CN 200810237970 A CN200810237970 A CN 200810237970A CN 101429018 A CN101429018 A CN 101429018A
- Authority
- CN
- China
- Prior art keywords
- aluminum garnet
- yttrium aluminum
- neodymium
- freezing
- doped yttrium
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Images
Landscapes
- Compositions Of Oxide Ceramics (AREA)
Abstract
The invention relates to a method for molding a neodymium-doped yttrium aluminum garnet transparent ceramic through refrigeration. The method comprises the following steps: selecting neodymium-doped yttrium aluminum garnet Nd:YAG powder as a raw material; adding the raw material powder and an organic dispersing agent to the mixed solution of water and glycerol; keeping stand, and then performing ball milling and ultrasonic vibration; adjusting the pH value of the slurry to between 8 and 10 with ammonia, and then pouring the slurry into a mold to be frozen for 8 to 12 hours; and performing vacuum drying and removing the mold to prepare a neodymium-doped YAG molded blank. The ceramic blank prepared by the method has high solid content, communication pores, and uniform ceramic blank density, thus the ceramic blank is not easy to deform in the subsequent processes of calcination and processing.
Description
Technical field
The invention belongs to laser ceramic material preparation technology, particularly a kind of freezing molding method of neodymium doped yttrium aluminum garnet transparent laser ceramic.
Background technology
Because ceramic laser medium preparation temperature is low, cost is low, can make the large size product, can realize high-dopant concentration, and is consuming time few, can be mass-produced, so caused the extensive attention of domestic and international researcher.Moulding process plays a part to form a connecting link in the preparation process of whole stupalith, is reliability, yield rate and the repeatable key that guarantees stupalith and parts, and is directly related with industrialization and large-scale production.Forming method has very large influence to the quality of ceramic body and the microstructure of sintered compact.
At present, for the forming method of yttrium aluminum garnet transparent ceramic, mainly contain following several: (1) is dry-pressing formed: the nano-powder after will sieving is pressed into disk with punching block under different pressure, obtain biscuit.On this basis, added the molding mode that waits static pressure, that is: earlier nano-powder is pressed into disk with punching block under the pressure of 50MPa, isostatic cool pressing (200MPa) obtains biscuit then.This blended molding mode has certain effect to reducing airtight air vent, and Shanghai Silicate Inst., Chinese Academy of Sciences has adopted this blended mode to obtain crystalline ceramics.But this method forms sealed porosity easily, and in the sintering process of postorder, pore is unfavorable for eliminating, thereby has influenced the optical quality of crystalline ceramics.(2) injection forming: this method is the common methods of traditional ceramics preparation.Injection forming mainly relies on capillary force action to remove solvent, forms to be communicated with pore.In the process of vacuum sintering, pore is discharged easily, obtains transparent laser ceramics easily.Japan has adopted the method for injection forming to prepare the uniform transparent laser ceramic of optical quality, yet the detailed process of injection forming is not described.In the process of injection forming, the slip that how to obtain uniform and stable and good fluidity just seems particularly important, and the patent and the bibliographical information of this respect are considerably less.On the basis of traditional injection forming, Muscovite scientist (Y.L.Kopylov et al., Opt.Mater. (2008)) adopt a kind of improved injection forming method---high-pressure slip-casting moulding (HPCSC) has prepared transparent laser ceramics.But the mode equipment complexity of this slip casing by pressure moulding, schedule of operation is loaded down with trivial details.All methods that relate to the injection forming of porous model all relate to the contact surface exclusion process that part moisture content is expected slurry and porous grinding tool, because the moisture content exclusion process occurs over just contact surface, make that the blank density after the moulding is inhomogeneous, make moulded products inconsistent because of the sintering contraction in sintering process easily, cause the distortion of pottery, and, because the partial density that base substrate contacts with plaster mould is higher, easy sintering during high temperature influences the eliminating of ceramic internal porosity, thereby causes ceramic transparency to descend.Simultaneously, the surface of moving to mould owing to the salt (calcium salt, sylvite, sodium salt) of solubility in the gypsum mold forms upper layer, can cause the variation of ceramic partially phase composite and the decline of optics and laser activity.
Summary of the invention
Problem and defective at the prior art existence, the invention provides a kind of freezing molding method of neodymium doped yttrium aluminum garnet transparent laser ceramic, adopt freezing injection forming preparation technology, make the neodymium-doped YAG base substrate of preparation can not produce the pore of sealing, this method is easy to near-net-shape, and promptly this method can be made and have profile and the akin formed body of purpose formed body shape.
A kind of freezing molding method of neodymium doped yttrium aluminum garnet transparent laser ceramic, step is as follows:
(1) select for use yttrium aluminum garnet (Nd:YAG) powder of doping neodymium to make raw material; Raw material powder and organic dispersing agent are joined in the mixing solutions of water and glycerol and leave standstill, time of repose is 12-24h, then its ball milling is mixed the back and forms slurry, and the ball milling time is 3-10h.;
Wherein: the dosage of organic dispersing agent is 1.0～1.5wt.% of raw material powder quality; The dosage of raw material powder is 60～65wt.% of each composition total mass; In the mixing solutions of water and glycerol, the mass ratio of water and glycerol is 9:1-12:1.
(2) slurry with step (1) preparation carries out ultrasonic vibrations, and the vibrations time is 5～8min, with ammoniacal liquor pH value of slurry is adjusted into 8～10, pour in the mould then, freezing 8～12h passed through vacuum-drying 24-36 hour again, removed to make behind the mould molding blank of neodymium-doped YAG.
The yttrium aluminum garnet general formula of the doping neodymium in the described step (1) is Nd
xY
3-xAl
5O
12, wherein, 0＜x≤0.5.
Organic dispersing agent in the described step (1) is preferably polyacrylic acid (PAA).
The moulding stock that uses in the described step (2) is tetrafluoroethylene.
Vacuum tightness in described step (2) process of vacuum drying is 50～80Pa.
Freezing temp in the described step (2) is preferably-40～-50 ℃.
Used neodymium-doped yttrium-aluminum garnet (Nd:YAG) powder of the present invention can prepare with Chinese patent file CN101311373 " a kind of method of synthetic YAG single crystal nano-powder ".
The forming method of the yttrium aluminum garnet transparent ceramic of doping neodymium provided by the invention, by adopting the Nd:YAG powder, the polyacrylic acid dispersant that adds some amount, adopting glycerol and water simultaneously is solvent, glycerol is believed to improve the heat transfer of slip, thereby forms uniform ceramic body microstructure.Adopt cryodesiccated mode, cryodesiccated cardinal principle is that water separates from solid by the method that distils, thereby has avoided because the hard aggregation that capillary force causes and breaking.
Adopt the base substrate of freeze-drying method preparation, eliminated the sealed porosity in the dry-pressing base substrate, simultaneously, the base substrate non-uniform phenomenon of having avoided porous model slip casting to bring again, the more important thing is, solved base substrate and contacted the pollution that brings, can improve the quality of molding blank, and overcome the ceramic mass problem that other forming method causes with gypsum grinding tool or metal grinding tool.The ceramic body that adopts the method preparation of freezing slip casting is that solid basis has been established in the preparation of later crystalline ceramics.
Description of drawings
Fig. 1 is the photo of the yttrium aluminum garnet ceramic body of the doping neodymium of employing the inventive method embodiment 1 preparation.
Fig. 2 is the microstructure photograph of the yttrium aluminum garnet ceramic body of the doping neodymium of employing the inventive method embodiment 1 preparation.
Embodiment
Following examples are to further specify of the present invention, but are not limited thereto.
Embodiment 1: a kind of forming method of yttrium aluminum garnet ceramic body of doping neodymium comprises the steps:
(1) with 20g Nd:YAG powder, put in the mixing solutions of 10.5ml water and glycerol, the mass ratio of water and glycerol is 9:1, the amount that adds polyacrylic acid dispersant is the 1.5wt.% of powder quality, raw material powder accounts for the 65wt.% of each composition (mixing solutions of water and glycerol, organic dispersing agent, raw material powder dosage sum) total mass, leave standstill 24h, put into planetary ball mill ball milling 6h;
(2) slurry behind the ball milling is poured out after, ultrasonic vibrations 5min, and be 8 with the pH that ammoniacal liquor is regulated slurry is poured into slurry in the tetrafluoroethylene mould, at-50 ℃ of freezing 10h, removes mould behind the vacuum-drying 24h.
Vacuum tightness in step (2) process of vacuum drying is 50Pa.
Embodiment 2:
(1) with 15g Nd:YAG powder, put in the mixing solutions of 8.2ml water and glycerol, the mass ratio of water and glycerol is 10.5:1, the amount that adds polyacrylic acid dispersant is the 1.4wt.% of powder quality, raw material powder accounts for the 64wt% of each composition total mass, leave standstill 24h, put into planetary ball mill ball milling 10h;
(2) slurry behind the ball milling is poured out after, ultrasonic vibrations 5min, and be 9 with the pH that ammoniacal liquor is regulated slurry is poured into slurry in the tetrafluoroethylene mould, at-40 ℃ of freezing 8h, removes mould behind the vacuum-drying 30h.
Vacuum tightness in step (2) process of vacuum drying is 60Pa.
Embodiment 3:
(1) with 30g Nd:YAG powder, put in the mixing solutions of 17.2ml water and glycerol, the mass ratio of water and glycerol is 12:1, the amount that adds polyacrylic acid dispersant is the 1.3wt.% of powder quality, raw material powder accounts for the 63wt% of each composition total mass, leave standstill 24h, put into planetary ball mill ball milling 10h;
(2) slurry behind the ball milling is poured out after, ultrasonic vibrations 5min, and be 10 with the pH that ammoniacal liquor is regulated slurry is poured into slurry in the tetrafluoroethylene mould, at-50 ℃ of freezing 12h, removes mould behind the vacuum-drying 36h.
Vacuum tightness in described step (2) process of vacuum drying is 80Pa.
Claims (6)
1. the freezing molding method of a neodymium doped yttrium aluminum garnet transparent laser ceramic is characterized in that step is as follows:
(1) select for use the yttrium aluminum garnet powder of doping neodymium to make raw material; Raw material powder and organic dispersing agent are joined in the mixing solutions of water and glycerol and leave standstill, time of repose is 12-24h, then its ball milling is mixed the back and forms slurry, and the ball milling time is 3-10h;
Wherein: the dosage of organic dispersing agent is 1.0～1.5wt.% of raw material powder quality; The quality of raw material powder is 60～65wt.% of each composition total mass;
(2) slurry with step (1) preparation carries out ultrasonic vibrations, and the vibrations time is 5～8min, with ammoniacal liquor pH value of slurry is adjusted into 8～10, pour in the mould then, freezing 8～12h passed through vacuum-drying 24-36 hour again, removed to make behind the mould molding blank of neodymium-doped YAG.
2. the freezing molding method of neodymium doped yttrium aluminum garnet transparent laser ceramic as claimed in claim 1, it is characterized in that: the organic dispersing agent in the described step (1) is preferably polyacrylic acid.
3. the freezing molding method of neodymium doped yttrium aluminum garnet transparent laser ceramic as claimed in claim 1, it is characterized in that: in the mixing solutions of described water of step (1) and glycerol, the mass ratio of water and glycerol is 9:1-12:1.
4. the freezing molding method of neodymium doped yttrium aluminum garnet transparent laser ceramic as claimed in claim 1 is characterized in that the moulding stock that uses in the described step (2) is tetrafluoroethylene.
5. the freezing molding method of neodymium doped yttrium aluminum garnet transparent laser ceramic as claimed in claim 1 is characterized in that the vacuum tightness in described step (2) process of vacuum drying is 50～80Pa.
6. the freezing molding method of neodymium doped yttrium aluminum garnet transparent laser ceramic as claimed in claim 1 is characterized in that the freezing temp in the described step (2) is preferably-40～-50 ℃.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2008102379708A CN101429018B (en) | 2008-12-04 | 2008-12-04 | Freezing molding method for neodymium doped yttrium aluminum garnet transparent laser ceramic |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2008102379708A CN101429018B (en) | 2008-12-04 | 2008-12-04 | Freezing molding method for neodymium doped yttrium aluminum garnet transparent laser ceramic |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN101429018A true CN101429018A (en) | 2009-05-13 |
| CN101429018B CN101429018B (en) | 2011-05-18 |
Family
ID=40644695
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2008102379708A Expired - Fee Related CN101429018B (en) | 2008-12-04 | 2008-12-04 | Freezing molding method for neodymium doped yttrium aluminum garnet transparent laser ceramic |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN101429018B (en) |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102173772A (en) * | 2010-12-27 | 2011-09-07 | 东北大学 | Synthesis method of yttrium aluminium garnet spherical powder or doped yttrium aluminium garnet spherical powder |
| CN102173800A (en) * | 2010-12-31 | 2011-09-07 | 中国科学院上海硅酸盐研究所 | Method for preparing yttrium aluminum garnet-based transparent ceramic by modifying of surface active agent |
| CN102173775A (en) * | 2011-02-23 | 2011-09-07 | 山东大学 | Method for preparing neodymium-doped yttrium aluminum garnet micro/nano powder by spray freeze-drying |
| CN104844212A (en) * | 2015-05-26 | 2015-08-19 | 中国工程物理研究院化工材料研究所 | Method for preparing yttrium aluminium garnet transparent ceramic |
| CN106083038A (en) * | 2016-06-16 | 2016-11-09 | 兰州理工大学 | A kind of Y TZP slurry preparation method for freeze forming |
| CN108530051A (en) * | 2018-03-20 | 2018-09-14 | 文华学院 | A method of being used to prepare nd yag doubled-frequency laser ceramic powder |
-
2008
- 2008-12-04 CN CN2008102379708A patent/CN101429018B/en not_active Expired - Fee Related
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102173772A (en) * | 2010-12-27 | 2011-09-07 | 东北大学 | Synthesis method of yttrium aluminium garnet spherical powder or doped yttrium aluminium garnet spherical powder |
| CN102173772B (en) * | 2010-12-27 | 2013-02-06 | 东北大学 | Synthesis method of yttrium aluminium garnet spherical powder or doped yttrium aluminium garnet spherical powder |
| CN102173800A (en) * | 2010-12-31 | 2011-09-07 | 中国科学院上海硅酸盐研究所 | Method for preparing yttrium aluminum garnet-based transparent ceramic by modifying of surface active agent |
| CN102173775A (en) * | 2011-02-23 | 2011-09-07 | 山东大学 | Method for preparing neodymium-doped yttrium aluminum garnet micro/nano powder by spray freeze-drying |
| CN104844212A (en) * | 2015-05-26 | 2015-08-19 | 中国工程物理研究院化工材料研究所 | Method for preparing yttrium aluminium garnet transparent ceramic |
| CN106083038A (en) * | 2016-06-16 | 2016-11-09 | 兰州理工大学 | A kind of Y TZP slurry preparation method for freeze forming |
| CN108530051A (en) * | 2018-03-20 | 2018-09-14 | 文华学院 | A method of being used to prepare nd yag doubled-frequency laser ceramic powder |
Also Published As
| Publication number | Publication date |
|---|---|
| CN101429018B (en) | 2011-05-18 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN101429018B (en) | Freezing molding method for neodymium doped yttrium aluminum garnet transparent laser ceramic | |
| CN101429050B (en) | Method for producing porous ceramic with oriented structure by employing freeze dehydration | |
| CN109516789A (en) | A kind of preparation method of the porous alumina ceramic based on Gyroid curved surface | |
| CN103833403B (en) | The preparation method of the toughness reinforcing boron carbide ceramics matrix material of a kind of silicon carbide whisker and product | |
| CN103360039A (en) | Large-size sheet-type electric-insulation heat-dissipation ceramic substrate and preparation method thereof | |
| CN110885244B (en) | Preparation method of yttrium aluminum garnet-based transparent ceramic optical fiber | |
| CN111393181B (en) | Preparation method of full-closed-pore porous mullite ceramic based on direct solidification injection molding | |
| CN101905481B (en) | Porous ceramic negative pressure slip casting device and method for preparing ceramic blank | |
| CN105384434B (en) | A kind of manufacture method of dry-pressing permanent-magnet ferrite | |
| CN104591702B (en) | A kind of LED highly heatproof and shockproof aluminium oxide ceramic substrate and manufacture method | |
| CN111270347A (en) | Method for preparing transparent ceramic optical fiber by gel injection molding | |
| CN102875132A (en) | Preparation method for large-size high-purity aluminum oxide ceramic material | |
| CN107914333A (en) | The method that zirconia ceramics cell phone rear cover is made using gel injection molding and forming technology | |
| CN105552212A (en) | 3-3 type piezoelectric ceramic/cement piezoelectric composite material and preparation method thereof | |
| CN101648814A (en) | Method for preparing high-performance ceramics by single-step solid phase reaction method | |
| CN105000890A (en) | Preparation method of large-size silicon nitride crucible | |
| CN100497256C (en) | Preparation method of compact ceramic of highly-oriented arrangement | |
| CN108000684A (en) | A kind of adhesive for powder injection forming preparation method and applications | |
| CN104451953A (en) | Preparation method of trivalent ytterbium ion doped lutetium-aluminum garnet transparent ceramic optical fibers | |
| CN102219477B (en) | Manufacture method for ceramic base of LED illuminating lamp | |
| CN110511021A (en) | A kind of novel zirconia ceramics forming method | |
| CN104478411A (en) | Method for preparing high-porosity in-situ grown magnesium borate whisker porous ceramics | |
| CN109437946A (en) | A kind of method that aqueous gel casting prepares YSZ fiber-based porous ceramic | |
| CN104230344A (en) | Low-temperature sintering preparation method of AlN ceramic added with multi-element sintering aid | |
| CN113372101A (en) | Preparation method of alumina ceramic |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| C17 | Cessation of patent right | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20110518 Termination date: 20131204 |