CN103864145B - Water quenching synthesizes the preparation technology of bar-shaped Zirconium powder - Google Patents
Water quenching synthesizes the preparation technology of bar-shaped Zirconium powder Download PDFInfo
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- CN103864145B CN103864145B CN201410115977.8A CN201410115977A CN103864145B CN 103864145 B CN103864145 B CN 103864145B CN 201410115977 A CN201410115977 A CN 201410115977A CN 103864145 B CN103864145 B CN 103864145B
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- Prior art keywords
- water quenching
- bar
- zirconium powder
- shaped zirconium
- shaped
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- 238000010791 quenching Methods 0.000 title claims abstract description 45
- 230000000171 quenching effect Effects 0.000 title claims abstract description 45
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 45
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 title claims abstract description 17
- 238000002360 preparation method Methods 0.000 title claims abstract description 7
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims abstract description 10
- 238000009413 insulation Methods 0.000 claims abstract description 7
- 239000002994 raw material Substances 0.000 claims abstract description 6
- 229910021529 ammonia Inorganic materials 0.000 claims abstract description 5
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims 1
- 229910052760 oxygen Inorganic materials 0.000 claims 1
- 239000001301 oxygen Substances 0.000 claims 1
- 229910052708 sodium Inorganic materials 0.000 claims 1
- 239000011734 sodium Substances 0.000 claims 1
- 239000000843 powder Substances 0.000 abstract description 11
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 abstract description 9
- DUNKXUFBGCUVQW-UHFFFAOYSA-J zirconium tetrachloride Chemical compound Cl[Zr](Cl)(Cl)Cl DUNKXUFBGCUVQW-UHFFFAOYSA-J 0.000 abstract description 5
- 239000012467 final product Substances 0.000 abstract description 4
- 238000000034 method Methods 0.000 abstract description 3
- 230000015572 biosynthetic process Effects 0.000 abstract description 2
- 238000003786 synthesis reaction Methods 0.000 abstract description 2
- 239000012254 powdered material Substances 0.000 abstract 1
- MCMNRKCIXSYSNV-UHFFFAOYSA-N ZrO2 Inorganic materials O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 9
- 239000000463 material Substances 0.000 description 9
- 239000002245 particle Substances 0.000 description 7
- 239000000919 ceramic Substances 0.000 description 6
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 description 6
- 230000003014 reinforcing effect Effects 0.000 description 5
- 229910001928 zirconium oxide Inorganic materials 0.000 description 5
- 230000035939 shock Effects 0.000 description 3
- 229910010293 ceramic material Inorganic materials 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 230000009466 transformation Effects 0.000 description 2
- 229910052581 Si3N4 Inorganic materials 0.000 description 1
- RKTYLMNFRDHKIL-UHFFFAOYSA-N copper;5,10,15,20-tetraphenylporphyrin-22,24-diide Chemical compound [Cu+2].C1=CC(C(=C2C=CC([N-]2)=C(C=2C=CC=CC=2)C=2C=CC(N=2)=C(C=2C=CC=CC=2)C2=CC=C3[N-]2)C=2C=CC=CC=2)=NC1=C3C1=CC=CC=C1 RKTYLMNFRDHKIL-UHFFFAOYSA-N 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 229910052574 oxide ceramic Inorganic materials 0.000 description 1
- 239000011224 oxide ceramic Substances 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- 239000000049 pigment Substances 0.000 description 1
- 239000011819 refractory material Substances 0.000 description 1
- 229910010271 silicon carbide Inorganic materials 0.000 description 1
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- RUDFQVOCFDJEEF-UHFFFAOYSA-N yttrium(III) oxide Inorganic materials [O-2].[O-2].[O-2].[Y+3].[Y+3] RUDFQVOCFDJEEF-UHFFFAOYSA-N 0.000 description 1
- 229910052726 zirconium Inorganic materials 0.000 description 1
Abstract
The present invention provides the preparation technology that a kind of water quenching synthesizes bar-shaped Zirconium powder, belongs to technical field of powdered material preparation.It is characterized in that：Using water quenching, with bar-shaped zirconium chloride powder as raw material, purity is more than 99%, 900~1100 DEG C of 0.2~1 h of insulation are heated to, water quenching, water quenching solution is sodium hydroxide solution or ammonia spirit, the pH value of water quenching solution is 8~10, water quenching solution temperature is 0~30 DEG C, is dried after water quenching, obtains final product bar-shaped Zirconium powder.Present invention process is simple, safe operation, low cost, 20 times or so of the bar-shaped Zirconium powder draw ratio of synthesis.
Description
Technical field
The present invention provides the preparation technology that a kind of water quenching synthesizes bar-shaped Zirconium powder, belongs to powder body material technology of preparing
Field.
Background technology
Zirconium dioxide is widely used in refractory material, ceramics due to its high temperature resistant, wear-resistant, corrosion resistant premium properties
The fields such as pigment, electronic ceramics, function ceramics and structural ceramics.In the research for having carried out, zirconium oxide is widely used in
The oxide ceramics such as aluminum oxide, and the non-oxide ceramicses such as silicon nitride, carborundum and zirconium boride toughness reinforcing, this mainly due to
The phase-change characteristic of zirconium oxide, when zirconium oxide from tetragonal phase converting be monoclinic phase when volume about expand 5%, the micro-flaw of generation
The toughness that can make material with residual stress is improved, therefore can be used to toughening ceramic.Conventional ceramic material is tough at present
Change method is mainly by adding toughness reinforcing mutually to improve the toughness of material, such as long fibre toughness reinforcing, crystal whisker toughened, ZrO2Phase transformation increases
Tough, sheet-like particle toughness reinforcing, rod-shpaed particle toughness reinforcing and yttria stabilizator etc..And bar-shaped zirconia particles not only have ZrO2Phase transformation
Toughening effect, also with rod-shpaed particle toughening effect.As zirconium oxide is in the continuous expansion of high-tech sector application, prepare different
The Zirconia particles of pattern have become the another focus of zirconium oxide research.
Meanwhile, rod-shpaed particle can improve the thermal shock resistance of material.The thermal shock resistance of material, refers mainly to material and bears
A certain degree of temperature drastically changes and ability that structure will not be destroyed, also known as thermal-shock resistance.Influence material thermal shock resistance
The principal element of energy has：Thermal coefficient of expansion, thermal conductivity factor, elastic modelling quantity, material inherent strength, fracture toughness of material etc..It is logical
Cross and prepare different-shape ceramic powder, such as piece, rod-shpaed particle, the shaking property of heat resistanceheat resistant of ceramic material can be improved.
And it is current, bar-shaped Zirconium powder there is no report.
The content of the invention
It is an object of the invention to provide a kind of process is simple, safe operation, low cost, it is easy to industrialization water quenching synthetic rod
The preparation technology of shape Zirconium powder, its technical scheme is：
Using water quenching, with bar-shaped zirconium chloride powder as raw material, purity is more than 99 %, is heated to 900~1100 DEG C of guarantors
0.2~1 h of temperature, water quenching, water quenching solution is sodium hydroxide solution or ammonia spirit, and the pH value of water quenching solution is 8~10, and water quenching is molten
Liquid temperature degree is 0~30 DEG C, is dried after water quenching, obtains final product bar-shaped Zirconium powder.
The present invention compared with prior art, has the following advantages that：
1st, the present invention uses water quenching, and safety simple to operate, efficiency high is conducive to industrialized production；
2nd, the bar-shaped Zirconium powder of present invention synthesis, with larger draw ratio, 20 times or so of draw ratio.
Brief description of the drawings
Fig. 1 is the XRD spectrums of powder after 900 DEG C of 1 h water quenchings of insulation of the present invention；
Fig. 2 is the SEM photograph of powder after 900 DEG C of 1 h water quenchings of insulation of the present invention.
Specific embodiment
Embodiment 1
Using water quenching, with bar-shaped zirconium chloride powder as raw material, purity is more than 99 %, is heated to 900 DEG C of 1 h of insulation,
Water quenching, water quenching solution is sodium hydroxide solution, and the pH value of water quenching solution is 10, and water quenching solution temperature is 0 DEG C, is dried after water quenching,
Obtain final product bar-shaped Zirconium powder.
Tested by XRD, it is seen that powder crystal type is monoclinic phase（See Fig. 1）；Tested by SEM, it is seen that zirconia powder
Body is bar-shaped, and a diameter of 10 μm or so, length is 200 μm or so（See Fig. 2）.
Embodiment 2
Using water quenching, with bar-shaped zirconium chloride powder as raw material, purity is more than 99 %, is heated to 1100 DEG C of insulations
0.2h, water quenching, water quenching solution is ammonia spirit, and the pH value of water quenching solution is 8, and water quenching solution temperature is 30 DEG C, is dried after water quenching,
Obtain final product bar-shaped Zirconium powder.
Embodiment 3
Using water quenching, with bar-shaped zirconium chloride powder as raw material, purity is more than 99 %, is heated to 1000 DEG C of insulations 0.5
H, water quenching, water quenching solution is ammonia spirit, and the pH value of water quenching solution is 9, and water quenching solution temperature is 20 DEG C, is dried after water quenching, i.e.,
Obtain bar-shaped Zirconium powder.
Claims (1)
1. a kind of water quenching synthesizes the preparation technology of bar-shaped Zirconium powder, it is characterised in that：Using water quenching, with bar-shaped tetrachloro
It is raw material to change zirconium powder body, and purity is more than 99 %, is heated to 900~1100 DEG C of 0.2~1 h of insulation, and water quenching, water quenching solution is hydrogen-oxygen
Change sodium solution or ammonia spirit, the pH values of water quenching solution are 8~10, and water quenching solution temperature is 0~30 DEG C, is dried after water quenching, i.e.,
Obtain bar-shaped Zirconium powder.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410115977.8A CN103864145B (en) | 2014-03-26 | 2014-03-26 | Water quenching synthesizes the preparation technology of bar-shaped Zirconium powder |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410115977.8A CN103864145B (en) | 2014-03-26 | 2014-03-26 | Water quenching synthesizes the preparation technology of bar-shaped Zirconium powder |
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| CN103864145A CN103864145A (en) | 2014-06-18 |
| CN103864145B true CN103864145B (en) | 2017-06-20 |
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Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3749763A (en) * | 1971-08-03 | 1973-07-31 | Humphreys Corp | Processing of silicate ores and product thereof |
Family Cites Families (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5978928A (en) * | 1982-10-25 | 1984-05-08 | Agency Of Ind Science & Technol | Manufacture of zirconia powder |
| JPH0233652B2 (en) * | 1986-03-11 | 1990-07-30 | Nippon Shokubai Kagaku Kogyo Kk | JIRUKONIAGANJUBIFUNMATSUNOSEIZOHOHO |
| CN101851005B (en) * | 2010-05-17 | 2011-08-31 | 山东理工大学 | Preparation method of high-dispersion zirconium oxide nano powder |
-
2014
- 2014-03-26 CN CN201410115977.8A patent/CN103864145B/en not_active Expired - Fee Related
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3749763A (en) * | 1971-08-03 | 1973-07-31 | Humphreys Corp | Processing of silicate ores and product thereof |
Non-Patent Citations (3)
| Title |
|---|
| Hydrothermal synthesis of crystallized nano-particles of rare earth-doped zirconia and hafnia;Masahiro Yoshimura et al.;《Materials Chemistry and Physics》;19991231;第61卷;第1-8页 * |
| 制备条件对ZrO2晶型的影响-四方ZrO2生成条件考察;韦薇;《天然气化工》;19991231;第24卷;第7-11页 * |
| 化学沉淀法制备纳米氧化锆的研究;王焕英等;《河北师范大学学报(自然科学版)》;20020930;第26卷(第5期);第488-491页 * |
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