CN106316392B - A kind of technique that environmentally protective semisolid method prepares yttrium zirconium powder body - Google Patents
A kind of technique that environmentally protective semisolid method prepares yttrium zirconium powder body Download PDFInfo
- Publication number
- CN106316392B CN106316392B CN201610789888.0A CN201610789888A CN106316392B CN 106316392 B CN106316392 B CN 106316392B CN 201610789888 A CN201610789888 A CN 201610789888A CN 106316392 B CN106316392 B CN 106316392B
- Authority
- CN
- China
- Prior art keywords
- yttrium
- zirconium
- powder body
- technique
- environmentally protective
- 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.)
- Active
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/48—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on zirconium or hafnium oxides, zirconates, zircon or hafnates
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
- C04B35/62605—Treating the starting powders individually or as mixtures
- C04B35/62625—Wet mixtures
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
- C04B35/62605—Treating the starting powders individually or as mixtures
- C04B35/62645—Thermal treatment of powders or mixtures thereof other than sintering
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/64—Burning or sintering processes
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3224—Rare earth oxide or oxide forming salts thereof, e.g. scandium oxide
- C04B2235/3225—Yttrium oxide or oxide-forming salts thereof
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Materials Engineering (AREA)
- Structural Engineering (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
- Composite Materials (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The invention belongs to rare earth field of compounding, the technique that a kind of environmentally protective semisolid method prepares yttrium zirconium powder body is provided, including following process flow: preparation, yttrium stabilization, zirconium stabilization, precipitating, hybrid reaction, the drying of zirconium solution roasts, milled, obtaining yttrium stabilised zirconia product.It can effectively ensure that in production process of the present invention using oxalic acid precipitation agent and do not generate waste water, reduce maturing temperature, process flow is short, and with short production cycle, equipment investment and its occupied area are few, reduce later period thermal decomposition temperature, reaches energy-efficient requirement.In addition, the mass-energy density of filler and the zirconium dioxide in zirconates ensures the structure of yttrium zirconium powder body in the present invention, production efficiency and quality are improved.
Description
Technical field
The invention belongs to rare earth field of compounding, in particular to a kind of environmentally protective semisolid method prepares the work of yttrium zirconium powder body
Skill.
Background technique
Zirconia ceramics, which has been obtained, to be widely applied, and by its excellent performance, is had become at present using most
One of wide oxide ceramics, most widely used toughened ceramic material are the cubic polycrystal zirconia (Y- of stabilized with yttrium oxide
TZP), yttrium stabilised zirconia is strong with heat resistanceheat resistant vibration property, high temperature resistant, chemical stability are good, Material cladding is prominent.
The method for preparing yttrium zirconium at present is broadly divided into wet chemical methods, solid phase the preparation method, gas-phase preparation method, wet chemical methods
The shortcomings that for preparation with washing process in generate a large amount of waste water (cl, NH4 containing high concentration+), cost of sewage disposal zirconium and pollution
Environment；The shortcomings that prepared by solid phase method is not easy uniformly for material, and particle is easy to reunite, and particle diameter distribution is wide；Vapor phase method prepares disadvantage
To be also easy to produce different byproducts and equipment valuableness, it is generally used for scientific research, unsuitable large-scale industrial production.
Summary of the invention
It is an object of the invention to solve upper technical problem, a kind of environmentally protective semisolid method is provided and prepares yttrium zirconium powder body
Technique.
Technical problem of the invention is mainly addressed by following technical proposals:
A kind of environmentally protective semisolid method prepares the technique of yttrium zirconium powder body, and specific technical solution is divided into following steps:
(1) preparation of zirconium solution: zirconates investment is dissolved equipped with stirring at normal temperature in the reaction kettle of solvent, stirring and dissolving is prepared
At 150~300g/l zirconium solution；
(2) yttrium is stablized: yttrium salt being put into reaction kettle, the molar ratio of yttrium and zirconium is 1:10~1:20, is continued stirring until
Material is uniformly mixed；Or the weight ratio of yttrium oxide and zirconium in zirconates is maintained at the section 1:5~1:20 in yttrium salt；
(3) filler stablizes (zirconium stablize): filler is put into reaction kettle, the quality and zirconates of filler its be converted to dioxy
The mass ratio for changing zirconium content is 1:1~1:9, to ensure the structure of yttrium zirconium powder body.Then dispersing agent is added, continues stirring until material
It is uniformly mixed；
(4) it precipitates: precipitating reagent is put into reaction kettle, precipitating reagent is added, zirconium yttrium is precipitated completely；
(5) hybrid reaction: after mixing is added in all materials, 1~6h is persistently stirred, so that material sufficiently reacts；
(6) drying roasting: material pp spoon made of step (5) is fitted into roasting pan, by calcining kiln 100~
300 DEG C of low temperature dryings, using the yttrium stabilised zirconia product for obtaining stable structure after 600~1000 DEG C of high-temperature roastings；
(7) acid mist that high-temperature calcination process generates is absorbed using acid fog absorption tower；
(8) increase milling work order, according to demand to reach different yttrium stabilised zirconia granularities.
Further, zirconates described in step (1) be zirconium carbonate, zirconium sulfate, zirconium oxychloride, zirconium nitrate any one.
Further, solvent described in step (1) be water, hydrochloric acid, sulfuric acid any one.
Further, yttrium salt described in step (2) be yttrium carbonate, yttrium oxalate, yttrium chloride any one.
Further, filler is zirconium dioxide in step (3).
Further, dispersing agent is pure water in step (3).
Further, precipitating reagent is oxalic acid in step (4).
Beneficial effects of the present invention: can effectively ensure that using oxalic acid precipitation agent in production process and do not generate waste water, drop
Low maturing temperature, process flow is short, with short production cycle, and equipment investment and its occupied area are few, reduces later period thermal decomposition temperature,
Reach energy-efficient requirement.In addition, the mass-energy density of filler and the zirconium dioxide in zirconates ensures the knot of yttrium zirconium powder body in the present invention
Structure improves production efficiency and quality.
Detailed description of the invention
Fig. 1 is process flow chart of the invention.
Specific embodiment
Below by embodiment, the technical solutions of the present invention will be further described.
Embodiment 1:
1. the preparation of zirconium solution: 150kg zirconium oxychloride being put into stirring at normal temperature in the 500l reaction kettle of dress solvent and is dissolved, is stirred
It mixes dissolution and is configured to zirconium solution 220g/l；2. yttrium is stablized: yttrium oxalate (conversion yttria levels are 7kg) is put into reaction kettle
In, it continues stirring until material and is uniformly mixed；3. filler is stablized: 10kg zirconia filler being put into reaction kettle, is persistently stirred
It mixes to material and is uniformly mixed；4. precipitating: 90kg precipitating reagent (oxalic acid) is put into reaction kettle, it is lasting to stir；5. hybrid reaction:
After mixing is added in all materials, 1~6h is persistently stirred, so that material sufficiently reacts.6. drying roasting: by the object in step 1.5
Material is put down, and is fitted into roasting pan with pp spoon, by 200 DEG C of low temperature drying 6h of electric calcining kiln, enters back into 800 DEG C of high temperature roastings of high temperature
The yttrium stabilised zirconia product of stable structure is obtained after burning 8h.7. the acid mist that high-temperature calcination process generates is absorbed using acid fog absorption tower.
8. milling work order can be increased according to customer demand, to reach the yttrium stabilised zirconia granularity of customer demand.
Embodiment 2:
1. the preparation of zirconium solution: 150kg zirconium carbonate is put into stirring at normal temperature in the 500l reaction kettle of dress solvent and is dissolved, stirring
Dissolution is configured to zirconium solution 200g/l；2. yttrium is stablized: yttrium carbonate (conversion yttria levels are 6kg) is put into reaction kettle,
Material is continued stirring until to be uniformly mixed；3. filler is stablized: 10kg zirconia filler being put into reaction kettle, is continued stirring until
Material is uniformly mixed；4. precipitating: 50kg precipitating reagent (oxalic acid) is put into reaction kettle, it is lasting to stir；5. hybrid reaction: all
After mixing is added in material, 1~6h is persistently stirred, so that material sufficiently reacts.6. drying roasting: the material in step 1.5 is put
Under, it is fitted into roasting pan with pp spoon, by 200 DEG C of low temperature drying 6h of electric calcining kiln, enters back into 800 DEG C of high-temperature roasting 8h of high temperature
The yttrium stabilised zirconia product of stable structure is obtained afterwards.7. the acid mist that high-temperature calcination process generates is absorbed using acid fog absorption tower.8. piece
Milling work order can be increased according to customer demand, to reach the yttrium stabilised zirconia granularity of customer demand.
Example applies 3:
1. the preparation of zirconium solution: 150kg zirconium oxychloride being put into stirring at normal temperature in the 500l reaction kettle of dress solvent and is dissolved, is stirred
It mixes dissolution and is configured to zirconium solution 280g/l；2. yttrium is stablized: yttrium chloride (conversion yttria levels are 7.5kg) is put into reaction kettle
In, it continues stirring until material and is uniformly mixed；3. filler is stablized: 10kg zirconia filler being put into reaction kettle, is persistently stirred
It mixes to material and is uniformly mixed；4. precipitating: 60kg precipitating reagent (oxalic acid) is put into reaction kettle, it is lasting to stir；5. hybrid reaction:
After mixing is added in all materials, 1~6h is persistently stirred, so that material sufficiently reacts.6. drying roasting: by the object in step 1.5
Material is put down, and is fitted into roasting pan with pp spoon, by 200 DEG C of low temperature drying 6h of electric calcining kiln, enters back into 800 DEG C of high temperature roastings of high temperature
The yttrium stabilised zirconia product of stable structure is obtained after burning 8h.7. the acid mist that high-temperature calcination process generates is absorbed using acid fog absorption tower.
8. milling work order can be increased according to customer demand, to reach the yttrium stabilised zirconia granularity of customer demand.
The present embodiment is the exemplary embodiment of the present invention, for those skilled in the art, in the present invention
On the basis of disclosing application method and principle, it is easy to make various types of improvement, be not limited solely to the above-mentioned tool of the present invention
Method described in body embodiment, structure, technique, therefore previously described mode is preferred embodiment, and and do not have limit
The meaning of property processed, it is all according to equivalence changes made by the present invention and modification, all model is protected in the range of claims of the present invention
In enclosing.
Claims (6)
1. a kind of technique that environmentally protective semisolid method prepares yttrium zirconium powder body, which comprises the following steps:
(1) preparation of zirconium solution: zirconates investment is dissolved equipped with stirring at normal temperature in the reaction kettle of solvent, stirring and dissolving is configured to
150~300g/l zirconium solution；
(2) yttrium is stablized: yttrium salt being put into reaction kettle, the molar ratio of yttrium and zirconium is 1:10~1:20, continues stirring until material
It is uniformly mixed；
(3) filler is stablized: filler is zirconium dioxide, and filler is put into reaction kettle, the quality and zirconates of filler its be converted to
The mass ratio of zirconium dioxide content is 1:1~1:5, and dispersing agent is then added, and continues stirring until material and is uniformly mixed；
(4) it precipitates: precipitating reagent is put into reaction kettle, precipitating reagent is added, zirconium yttrium is precipitated completely；
(5) hybrid reaction: after mixing is added in all materials, 1~6h is persistently stirred, so that material sufficiently reacts；
(6) drying roasting: material pp spoon made of step (5) is fitted into roasting pan, by 100~300 DEG C of calcining kiln
Low temperature drying, using the yttrium stabilised zirconia product for obtaining stable structure after 600~1000 DEG C of high-temperature roastings；
(7) acid mist that high-temperature calcination process generates is absorbed using acid fog absorption tower；
(8) increase milling work order, according to demand to reach different yttrium stabilised zirconia granularities.
2. the technique that a kind of environmentally protective semisolid method according to claim 1 prepares yttrium zirconium powder body, which is characterized in that step
Suddenly zirconates described in (1) be zirconium carbonate, zirconium sulfate, zirconium oxychloride, zirconium nitrate any one.
3. the technique that a kind of environmentally protective semisolid method according to claim 1 prepares yttrium zirconium powder body, which is characterized in that step
Suddenly solvent described in (1) be water, hydrochloric acid, sulfuric acid any one.
4. the technique that a kind of environmentally protective semisolid method according to claim 1 prepares yttrium zirconium powder body, which is characterized in that step
Suddenly yttrium salt described in (2) be yttrium carbonate, yttrium oxalate, yttrium chloride any one.
5. the technique that a kind of environmentally protective semisolid method according to claim 1 prepares yttrium zirconium powder body, which is characterized in that step
Suddenly dispersing agent is pure water in (3).
6. the technique that a kind of environmentally protective semisolid method according to claim 1 prepares yttrium zirconium powder body, which is characterized in that step
Suddenly precipitating reagent is oxalic acid in (4).
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610789888.0A CN106316392B (en) | 2016-08-30 | 2016-08-30 | A kind of technique that environmentally protective semisolid method prepares yttrium zirconium powder body |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610789888.0A CN106316392B (en) | 2016-08-30 | 2016-08-30 | A kind of technique that environmentally protective semisolid method prepares yttrium zirconium powder body |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN106316392A CN106316392A (en) | 2017-01-11 |
| CN106316392B true CN106316392B (en) | 2019-04-12 |
Family
ID=57789217
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201610789888.0A Active CN106316392B (en) | 2016-08-30 | 2016-08-30 | A kind of technique that environmentally protective semisolid method prepares yttrium zirconium powder body |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN106316392B (en) |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5122317A (en) * | 1990-01-12 | 1992-06-16 | The Regents Of The University Of Michigan | Method of superplastically deforming zirconia materials |
| CN101628733A (en) * | 2008-07-14 | 2010-01-20 | 东北大学 | Method for preparing magnesia partially-stabilized monoclinic zirconia powder under normal pressure and at low temperature |
| CN101993248A (en) * | 2009-08-10 | 2011-03-30 | 上海锦奕新材料科技有限公司 | Additive for sintering yttrium-stabilized zirconia at low temperature |
-
2016
- 2016-08-30 CN CN201610789888.0A patent/CN106316392B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5122317A (en) * | 1990-01-12 | 1992-06-16 | The Regents Of The University Of Michigan | Method of superplastically deforming zirconia materials |
| CN101628733A (en) * | 2008-07-14 | 2010-01-20 | 东北大学 | Method for preparing magnesia partially-stabilized monoclinic zirconia powder under normal pressure and at low temperature |
| CN101993248A (en) * | 2009-08-10 | 2011-03-30 | 上海锦奕新材料科技有限公司 | Additive for sintering yttrium-stabilized zirconia at low temperature |
Also Published As
| Publication number | Publication date |
|---|---|
| CN106316392A (en) | 2017-01-11 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN104003697B (en) | A kind of preparation method of BSAS composite ceramic powder | |
| CN101507917A (en) | Solid base catalyst for synthesizing alkanolamide type compound and preparation method thereof | |
| CN101024514A (en) | Novel process for preparing cubic-phase nano zirconium dioxide | |
| CN103539210A (en) | Preparation method of cobalt molybdate microcrystals | |
| CN104671797B (en) | Internal gelation method for ceramic microspheres capable of keeping gel solution steady at normal temperature | |
| CN106276960A (en) | A kind of method of flyash microwave alkali fusion Hydrothermal Synthesis faujasite | |
| CN105883886B (en) | A kind of method that high-purity αsemiwatergypsum powder is prepared using salt chemical engineering accessory substance | |
| CN104788034B (en) | A kind of preparation method of the long-acting swelling agent of ardealite base high energy | |
| CN107129169A (en) | A kind of preparation method of magnesium oxysulfide concrete | |
| CN104003715A (en) | ZrC-ZrO2 composite ceramic microsphere and preparation method thereof | |
| CN109369182A (en) | A kind of preparation method of cubic phase garnet solid electrolyte material | |
| CN103833066B (en) | Preparation method for plate-type copper nitrate basic | |
| CN103979567B (en) | A kind of low-temperature growth CrB or CrB 2the method of powder | |
| CN102718258A (en) | Preparation method of Gd2Zr2O7 nano-powder | |
| CN107162450A (en) | A kind of magnesium oxysulfide concrete | |
| CN105905944A (en) | Method of preparing Bi2Zr2O7 nano material through non-hydrolytic sol-gel method | |
| CN106316392B (en) | A kind of technique that environmentally protective semisolid method prepares yttrium zirconium powder body | |
| CN107188150A (en) | A kind of preparation method of Mesoporous zirconium phosphate | |
| CN105460918A (en) | Preparation method of hollow carbon sphere | |
| CN105460983A (en) | Method for preparing nickel cobaltate nano material for super capacitor | |
| CN104071845B (en) | A kind of SLTON perovskite typed oxynitride raw powder's production technology | |
| CN106186036B (en) | A kind of preparation method of hexagon cerium dioxide nano sheet material | |
| CN104086181B (en) | The preparation method of SLMTON perovskite typed oxynitride solid-solution powder | |
| CN100447091C (en) | Synthesis process of mesoporous ZrO2 molecular sieve | |
| CN103708549B (en) | Nano level ZrO 2the preparation method of powder |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant | ||
| PP01 | Preservation of patent right | ||
| PP01 | Preservation of patent right |
Effective date of registration: 20230323 Granted publication date: 20190412 |