CN109251035A - One kind (Zr, Hf) B2The preparation method of ceramic powder - Google Patents
One kind (Zr, Hf) B2The preparation method of ceramic powder Download PDFInfo
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- 229910052735 hafnium Inorganic materials 0.000 title claims abstract description 132
- 229910052726 zirconium Inorganic materials 0.000 title claims abstract description 127
- 239000000843 powder Substances 0.000 title claims abstract description 111
- 239000000919 ceramic Substances 0.000 title claims abstract description 65
- 238000002360 preparation method Methods 0.000 title claims abstract description 46
- 150000001875 compounds Chemical class 0.000 claims abstract description 108
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims abstract description 87
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 claims abstract description 84
- WMFOQBRAJBCJND-UHFFFAOYSA-M Lithium hydroxide Chemical compound [Li+].[OH-] WMFOQBRAJBCJND-UHFFFAOYSA-M 0.000 claims abstract description 84
- 229910052796 boron Inorganic materials 0.000 claims abstract description 84
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical group [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 75
- 150000003839 salts Chemical class 0.000 claims abstract description 63
- 239000003638 chemical reducing agent Substances 0.000 claims abstract description 57
- 229910052783 alkali metal Inorganic materials 0.000 claims abstract description 50
- 150000001340 alkali metals Chemical class 0.000 claims abstract description 50
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims abstract description 38
- 239000004111 Potassium silicate Substances 0.000 claims abstract description 22
- 239000004115 Sodium Silicate Substances 0.000 claims abstract description 22
- FZQSLXQPHPOTHG-UHFFFAOYSA-N [K+].[K+].O1B([O-])OB2OB([O-])OB1O2 Chemical compound [K+].[K+].O1B([O-])OB2OB([O-])OB1O2 FZQSLXQPHPOTHG-UHFFFAOYSA-N 0.000 claims abstract description 21
- 229910021538 borax Inorganic materials 0.000 claims abstract description 21
- PSHMSSXLYVAENJ-UHFFFAOYSA-N dilithium;[oxido(oxoboranyloxy)boranyl]oxy-oxoboranyloxyborinate Chemical compound [Li+].[Li+].O=BOB([O-])OB([O-])OB=O PSHMSSXLYVAENJ-UHFFFAOYSA-N 0.000 claims abstract description 21
- UQGFMSUEHSUPRD-UHFFFAOYSA-N disodium;3,7-dioxido-2,4,6,8,9-pentaoxa-1,3,5,7-tetraborabicyclo[3.3.1]nonane Chemical compound [Na+].[Na+].O1B([O-])OB2OB([O-])OB1O2 UQGFMSUEHSUPRD-UHFFFAOYSA-N 0.000 claims abstract description 21
- 239000004328 sodium tetraborate Substances 0.000 claims abstract description 21
- 235000010339 sodium tetraborate Nutrition 0.000 claims abstract description 21
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 claims abstract description 20
- 239000004327 boric acid Substances 0.000 claims abstract description 20
- ANBBXQWFNXMHLD-UHFFFAOYSA-N aluminum;sodium;oxygen(2-) Chemical compound [O-2].[O-2].[Na+].[Al+3] ANBBXQWFNXMHLD-UHFFFAOYSA-N 0.000 claims abstract description 19
- XGZVUEUWXADBQD-UHFFFAOYSA-L lithium carbonate Chemical compound [Li+].[Li+].[O-]C([O-])=O XGZVUEUWXADBQD-UHFFFAOYSA-L 0.000 claims abstract description 19
- 229910052808 lithium carbonate Inorganic materials 0.000 claims abstract description 19
- PAZHGORSDKKUPI-UHFFFAOYSA-N lithium metasilicate Chemical compound [Li+].[Li+].[O-][Si]([O-])=O PAZHGORSDKKUPI-UHFFFAOYSA-N 0.000 claims abstract description 19
- 229910052912 lithium silicate Inorganic materials 0.000 claims abstract description 19
- NNHHDJVEYQHLHG-UHFFFAOYSA-N potassium silicate Chemical compound [K+].[K+].[O-][Si]([O-])=O NNHHDJVEYQHLHG-UHFFFAOYSA-N 0.000 claims abstract description 19
- 229910052913 potassium silicate Inorganic materials 0.000 claims abstract description 19
- 235000019353 potassium silicate Nutrition 0.000 claims abstract description 19
- 229910001388 sodium aluminate Inorganic materials 0.000 claims abstract description 19
- 229910000029 sodium carbonate Inorganic materials 0.000 claims abstract description 19
- 235000019795 sodium metasilicate Nutrition 0.000 claims abstract description 19
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 claims abstract description 19
- 229910052911 sodium silicate Inorganic materials 0.000 claims abstract description 19
- 230000001681 protective effect Effects 0.000 claims abstract description 18
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 16
- 239000011863 silicon-based powder Substances 0.000 claims abstract description 16
- 239000004411 aluminium Substances 0.000 claims abstract description 15
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims abstract description 15
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 15
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 12
- 229910052751 metal Inorganic materials 0.000 claims abstract description 10
- 239000002184 metal Substances 0.000 claims abstract description 10
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Chemical compound [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 claims abstract 4
- 229910000027 potassium carbonate Inorganic materials 0.000 claims abstract 2
- 239000000203 mixture Substances 0.000 claims description 31
- 239000007864 aqueous solution Substances 0.000 claims description 29
- 239000011734 sodium Substances 0.000 claims description 4
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 claims description 3
- 239000003513 alkali Substances 0.000 claims description 3
- 229910052744 lithium Inorganic materials 0.000 claims description 3
- 239000000243 solution Substances 0.000 claims description 2
- 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
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims 1
- 239000010931 gold Substances 0.000 claims 1
- 229910052737 gold Inorganic materials 0.000 claims 1
- 239000001257 hydrogen Substances 0.000 claims 1
- 229910052739 hydrogen Inorganic materials 0.000 claims 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 claims 1
- 229910001947 lithium oxide Inorganic materials 0.000 claims 1
- 229910052708 sodium Inorganic materials 0.000 claims 1
- 238000004519 manufacturing process Methods 0.000 abstract description 9
- 239000002245 particle Substances 0.000 abstract description 8
- 238000009826 distribution Methods 0.000 abstract description 5
- 238000005406 washing Methods 0.000 abstract description 2
- 239000004615 ingredient Substances 0.000 abstract 1
- 239000000126 substance Substances 0.000 description 37
- 235000011121 sodium hydroxide Nutrition 0.000 description 26
- 238000000034 method Methods 0.000 description 22
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 17
- BVKZGUZCCUSVTD-UHFFFAOYSA-N carbonic acid Chemical compound OC(O)=O BVKZGUZCCUSVTD-UHFFFAOYSA-N 0.000 description 17
- 229910052700 potassium Inorganic materials 0.000 description 17
- 239000011591 potassium Substances 0.000 description 17
- 235000011118 potassium hydroxide Nutrition 0.000 description 17
- 235000017550 sodium carbonate Nutrition 0.000 description 17
- 238000006243 chemical reaction Methods 0.000 description 13
- 150000001339 alkali metal compounds Chemical class 0.000 description 12
- 238000003786 synthesis reaction Methods 0.000 description 10
- 230000015572 biosynthetic process Effects 0.000 description 9
- 238000006722 reduction reaction Methods 0.000 description 9
- 238000002156 mixing Methods 0.000 description 8
- 239000002994 raw material Substances 0.000 description 5
- 238000004140 cleaning Methods 0.000 description 4
- 239000007791 liquid phase Substances 0.000 description 4
- 239000000047 product Substances 0.000 description 4
- 238000001228 spectrum Methods 0.000 description 4
- 239000002253 acid Substances 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 239000011777 magnesium Substances 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 2
- 239000006227 byproduct Substances 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- JKWMSGQKBLHBQQ-UHFFFAOYSA-N diboron trioxide Chemical compound O=BOB=O JKWMSGQKBLHBQQ-UHFFFAOYSA-N 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 229910052749 magnesium Inorganic materials 0.000 description 2
- 239000012071 phase Substances 0.000 description 2
- 229910052573 porcelain Inorganic materials 0.000 description 2
- 238000011084 recovery Methods 0.000 description 2
- 229910052580 B4C Inorganic materials 0.000 description 1
- 206010054949 Metaplasia Diseases 0.000 description 1
- 229910007948 ZrB2 Inorganic materials 0.000 description 1
- 238000010306 acid treatment Methods 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- INAHAJYZKVIDIZ-UHFFFAOYSA-N boron carbide Chemical compound B12B3B4C32B41 INAHAJYZKVIDIZ-UHFFFAOYSA-N 0.000 description 1
- VWZIXVXBCBBRGP-UHFFFAOYSA-N boron;zirconium Chemical compound B#[Zr]#B VWZIXVXBCBBRGP-UHFFFAOYSA-N 0.000 description 1
- 239000011195 cermet Substances 0.000 description 1
- HPNSNYBUADCFDR-UHFFFAOYSA-N chromafenozide Chemical compound CC1=CC(C)=CC(C(=O)N(NC(=O)C=2C(=C3CCCOC3=CC=2)C)C(C)(C)C)=C1 HPNSNYBUADCFDR-UHFFFAOYSA-N 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 230000015689 metaplastic ossification Effects 0.000 description 1
- 239000003595 mist Substances 0.000 description 1
- 230000001902 propagating effect Effects 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 230000036632 reaction speed Effects 0.000 description 1
- 238000002791 soaking Methods 0.000 description 1
- 238000010189 synthetic method Methods 0.000 description 1
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
- C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
- C04B35/58—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides
- C04B35/5805—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides based on borides
- C04B35/58064—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides based on borides based on refractory borides
- C04B35/58078—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides based on borides based on refractory borides based on zirconium or hafnium borides
-
- 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
-
- 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
- C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
- C04B2235/74—Physical characteristics
- C04B2235/78—Grain sizes and shapes, product microstructures, e.g. acicular grains, equiaxed grains, platelet-structures
- C04B2235/781—Nanograined materials, i.e. having grain sizes below 100 nm
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)
- Silicates, Zeolites, And Molecular Sieves (AREA)
- Compositions Of Oxide Ceramics (AREA)
- Silicon Compounds (AREA)
Abstract
The present invention relates to one kind (Zr, Hf) B2The preparation method of ceramic powder.Technical solution is: by reducing agent: containing (Zr; Hf) compound: boron source: the mass ratio of alkali metal-containing compound fused salt is 1.0: (1.0~5.0): (0.7~4.0): (0.2~18.0) ingredient; it mixes; it is dry, it is heat-treated 0.5~8h under the conditions of protective atmosphere and 600~1300 DEG C, is dissolved with water or aqueous slkali; washing; it is dry, (Zr, Hf) B is made2Ceramic powder.Wherein: reducing agent is more than one in silicon powder and aluminium powder；It is metal (Zr, Hf) powder and (Zr, Hf) containing (Zr, Hf) compound2More than one in powder；Boron source is boron cash, boric acid, sodium tetraborate, dipotassium tetraborate, more than one in lithium tetraborate；Alkali metal-containing compound fused salt is sodium hydroxide, sodium metasilicate, sodium carbonate, potassium hydroxide, potassium silicate, potassium carbonate, lithium hydroxide, lithium metasilicate, lithium carbonate, more than one in sodium aluminate.The present invention is at low cost, environmental-friendly and easy to industrialized production, and made product granularity is small and narrow particle size distribution.
Description
Technical field
The invention belongs to boride ceramics powder technology fields.More particularly to one kind (Zr, Hf) B2The preparation of ceramic powder
Method.
Background technique
(Zr,Hf)B2With high-melting-point, high rigidity, high intensity, good thermally conductive and excellent wear-resisting property.It makes pottery in conduction
The neck such as porcelain, ceramic cutter, mold, metallurgical ceramic crucible, high temperature exothermic element, cermet and ceramic matric composite
Domain has a wide range of applications.(Zr,Hf)B2Sill has excellent mechanics, ermal physics, chemistry and frictional behaviour, can be in the limit
It is on active service under environment, such as the leading edge of hypersonic aircraft nose cone, wing and empennage.
Particle size, particle diameter distribution, reunion and purity of powder etc. be characterized in influence ceramic performance it is crucial because
One of element, high-performance (Zr, Hf) B2The synthesis and preparation of ceramic powder are one of current research hot spots.
(Zr,Hf)B2The preparation method of ceramic powder has more document report, also such as element direct synthesis technique, boron heat
Original, carbon thermal reduction, self-propagating high-temperature synthesis etc..Element direct synthesis technique is with metal (Zr, Hf) and pure boron, in atmosphere protection
Lower high temperature directly reacts synthesis, and the powder purity of this method synthesis is higher.Boron thermal reduction method is (Zr, Hf) B2The common conjunction of powder
It is to restore (Zr, Hf) O using pure boron or boron carbide as reducing agent at one of method2Powder can obtain grain by this method
(Zr, the Hf) B of diameter less than 1 μm2Ceramic powder.The powder purity of above two method synthesis is higher, but cost of material is higher.Carbon
Thermal reduction is to restore B using C as reducing agent2O3(Zr, Hf) O2Powder, though this method simple process, cost is relatively low and be suitable for
Industrialized production, but this method synthesis temperature is high, soaking time is long, and diameter of particle obtained is compared with thick, impurity more (Yang Lei, grandson
Quiet, Gui Tao waits additive to prepare ZrB to carbothermic reduction reaction2Influence [J] rare metal of partial size and pattern, 2017 (12):
1352-1358.).The synthesis of self-propagating high-temperature method is with (Zr, Hf) or (Zr, Hf) O2、B2O3Or H3BO3For raw material, metal Mg is also
Former agent, by magnesium thermit cause system self-propagating reaction, though this method have reaction speed is fast, the time is short, energy consumption is small and
The high advantage of yield, but the difficult accurate control of powder size obtained, pattern, more (the Zhang Tianmei self- propagating magnesium of product impurity content
Thermal reduction preparation high-purity zirconium diboride micro mist [D] Harbin Institute of Technology, 2006.).
In summary it analyzes, existing (Zr, Hf) B2The synthetic method of ceramic powder there is a problem of different degrees of: raw material at
This is high, and reaction temperature is higher, (Zr, Hf) B of synthesis2Ceramic powder size be difficult to control, activity it is lower, product powder it is miscellaneous
Matter content is more high-leveled and difficult with removal, and environmental pollution is serious for subsequent acid treatment and purification purifying technique.
Summary of the invention
The present invention is directed to overcome prior art defect, provide that a kind of raw material is easy to get, simple process, production cost are low, environment
Friendly and easy to industrialized production (Zr, Hf) B2The preparation method of ceramic powder.
To achieve the above object, the technical solution adopted by the present invention is that: press reducing agent: contain (Zr, Hf) compound: boron source:
The mass ratio of alkali metal-containing compound fused salt is 1.0: (1.0~5.0): (0.7~4.0): and (0.2~18.0), by the reduction
Agent, described uniformly mixed containing (Zr, Hf) compound, the boron source and the alkali metal-containing compound fused salt, drying, in protectiveness
It is heat-treated 0.5~8h under the conditions of atmosphere and 600~1300 DEG C, is then dissolved under the conditions of room temperature~250 DEG C with water or aqueous slkali,
Washing, it is dry, (Zr, Hf) B is made2Ceramic powder.
The reducing agent be silicon powder or be aluminium powder or be silicon powder and aluminium powder mixture.
(Zr, the Hf) compound that contains is metal (Zr, Hf) powder and (Zr, Hf) O2One or more of powder.
The boron source is one or more of boron cash, boric acid, sodium tetraborate, dipotassium tetraborate and lithium tetraborate.
The alkali metal-containing compound fused salt is sodium hydroxide, sodium metasilicate, sodium carbonate, potassium hydroxide, potassium silicate, carbonic acid
One or more of potassium, lithium hydroxide, lithium metasilicate, lithium carbonate and sodium aluminate.
The aqueous slkali be one of sodium hydrate aqueous solution, potassium hydroxide aqueous solution and lithium hydroxide aqueous solution with
On.
SiO in the sodium metasilicate2With Na2Molar ratio≤1 of O.
SiO in the potassium silicate2With K2Molar ratio≤1 of O.
SiO in the lithium metasilicate2With Li2Molar ratio≤1 of O.
Due to the adoption of the above technical scheme, the present invention has following good effect compared with prior art:
(1) present invention in the reaction system introduce alkali metal-containing compound fused salt, alkali metal-containing compound fused salt can compared with
Liquid phase is formed at a temperature of low, strengthens mass transport process, improves the dynamic conditions of chemical reaction, improves reduction reaction efficiency；And
Reaction carries out in the liquid phase, and reaction condition is mild, (Zr, Hf) B of generation2Ceramic powder has partial size small, narrow particle size distribution
Feature.
(2) present invention boron-containing compounds such as boric acid, sodium tetraborate, dipotassium tetraborate, lithium tetraborate can be used to make in addition to boric anhydride
For boron source, raw material sources are widened, production cost is low.
(3) the alkali metal-containing compound fused salt that the present invention uses can participate in chemically reacting, and improve the thermodynamics of chemical reaction
Condition promotes the progress of reduction reaction, improves yield and the rate of recovery.Product after heat treatment is directly washed or alkali cleaning, technique letter
Single, byproduct recoverable avoids traditional acid cleaning process and causes the drawbacks of seriously polluting to environment, environmental-friendly, be easy to
Industrialized production.
Therefore, the present invention has the characteristics that lower production costs, environmental-friendly, easy to industrialized production, obtained (Zr,
Hf)B2Ceramic powder has the characteristics that partial size is small, narrow particle size distribution.
Detailed description of the invention
Fig. 1 is one kind (Zr, Hf) B prepared by the present invention2The XRD spectrum of ceramic powder；
Fig. 2 is (Zr, Hf) B shown in Fig. 12The SEM photograph of ceramic powder；
Fig. 3 is another kind (Zr, Hf) B prepared by the present invention2The XRD spectrum of ceramic powder.
Specific embodiment
In order to better understand the present invention, what the present invention is further explained with reference to the accompanying drawings and detailed description is interior
Hold, but the present invention is not limited solely to present embodiment.
It is first that technical parameter Unify legislation involved in present embodiment is as follows to avoid repeating, in embodiment not
It repeats again:
SiO in the sodium metasilicate2With Na2Molar ratio≤1 of O.
SiO in the potassium silicate2With K2Molar ratio≤1 of O.
SiO in the lithium metasilicate2With Li2Molar ratio≤1 of O.
Embodiment 1
One kind (Zr, Hf) B2The preparation method of ceramic powder.Preparation method described in the present embodiment is:
By reducing agent: contain (Zr, Hf) compound: boron source: the mass ratio of alkali metal-containing compound fused salt is 1.0: (1.0~
2.5): (0.7~1.5): (0.2~5.0) by the reducing agent, described containing (Zr, Hf) compound, the boron source and described contains
Alkali metal compound fused salt is uniformly mixed, dry, 6~8h is heat-treated under the conditions of protective atmosphere and 1000~1300 DEG C, so
It is dissolved, is washed under the conditions of 95~200 DEG C with aqueous slkali afterwards, it is dry, (Zr, Hf) B is made2Ceramic powder.
The reducing agent is silicon powder.
(Zr, the Hf) compound that contains is (Zr, Hf) O2Powder.
The boron source is any one substance in boron cash, boric acid, sodium tetraborate, dipotassium tetraborate and lithium tetraborate.
The alkali metal-containing compound fused salt is sodium hydroxide, sodium metasilicate, sodium carbonate, potassium hydroxide, potassium silicate, carbonic acid
Any one substance in potassium, lithium hydroxide, lithium metasilicate, lithium carbonate and sodium aluminate.
The aqueous slkali is two kinds or more in sodium hydrate aqueous solution, potassium hydroxide aqueous solution and lithium hydroxide aqueous solution
Mixture.
Embodiment 2
One kind (Zr, Hf) B2The preparation method of ceramic powder.Preparation method described in the present embodiment is:
By reducing agent: contain (Zr, Hf) compound: boron source: the mass ratio of alkali metal-containing compound fused salt is 1.0: (1.0~
2.5): (0.7~1.5): (0.2~5.0) by the reducing agent, described containing (Zr, Hf) compound, the boron source and described contains
Alkali metal compound fused salt is uniformly mixed, dry, 6~8h is heat-treated under the conditions of protective atmosphere and 1000~1300 DEG C, so
It is dissolved, is washed under the conditions of 95~200 DEG C with water afterwards, it is dry, (Zr, Hf) B is made2Ceramic powder.
The reducing agent is aluminium powder.
(Zr, the Hf) compound that contains is (Zr, Hf) O2Powder.
The boron source is any two material mixing in boron cash, boric acid, sodium tetraborate, dipotassium tetraborate and lithium tetraborate
Object.
The alkali metal-containing compound fused salt is sodium hydroxide, sodium metasilicate, sodium carbonate, potassium hydroxide, potassium silicate, carbonic acid
The mixture of any two substance in potassium, lithium hydroxide, lithium metasilicate, lithium carbonate and sodium aluminate.
Embodiment 3
One kind (Zr, Hf) B2The preparation method of ceramic powder.Preparation method described in the present embodiment is:
By reducing agent: contain (Zr, Hf) compound: boron source: the mass ratio of alkali metal-containing compound fused salt is 1.0: (1.0~
2.5): (0.7~1.5): (0.2~5.0) by the reducing agent, described containing (Zr, Hf) compound, the boron source and described contains
Alkali metal compound fused salt is uniformly mixed, dry, 6~8h is heat-treated under the conditions of protective atmosphere and 1000~1300 DEG C, so
It is dissolved, is washed under the conditions of 95~200 DEG C with water afterwards, it is dry, (Zr, Hf) B is made2Ceramic powder.
The reducing agent is the mixture of silicon powder and aluminium powder.
(Zr, the Hf) compound that contains is metal (Zr, Hf) powder.
The boron source is any three kinds of material mixings in boron cash, boric acid, sodium tetraborate, dipotassium tetraborate and lithium tetraborate
Object.
The alkali metal-containing compound fused salt is sodium hydroxide, sodium metasilicate, sodium carbonate, potassium hydroxide, potassium silicate, carbonic acid
The mixture of any three kinds of substances in potassium, lithium hydroxide, lithium metasilicate, lithium carbonate and sodium aluminate.
Embodiment 4
One kind (Zr, Hf) B2The preparation method of ceramic powder.Preparation method described in the present embodiment is:
By reducing agent: contain (Zr, Hf) compound: boron source: the mass ratio of alkali metal-containing compound fused salt is 1.0: (1.0~
2.5): (0.7~1.5): (0.2~5.0) by the reducing agent, described containing (Zr, Hf) compound, the boron source and described contains
Alkali metal compound fused salt is uniformly mixed, dry, 6~8h is heat-treated under the conditions of protective atmosphere and 1000~1300 DEG C, so
It is dissolved, is washed under the conditions of 95~200 DEG C with aqueous slkali afterwards, it is dry, (Zr, Hf) B is made2Ceramic powder.
The reducing agent is silicon powder.
(Zr, the Hf) compound that contains is (Zr, Hf) powder and (Zr, Hf) O2The mixture of powder.
The boron source is the above substance of any four in boron cash, boric acid, sodium tetraborate, dipotassium tetraborate and lithium tetraborate
Mixture.
The alkali metal-containing compound fused salt is sodium hydroxide, sodium metasilicate, sodium carbonate, potassium hydroxide, potassium silicate, carbonic acid
The mixture of the above substance of any four in potassium, lithium hydroxide, lithium metasilicate, lithium carbonate and sodium aluminate.
The aqueous slkali is any one in sodium hydrate aqueous solution, potassium hydroxide aqueous solution and lithium hydroxide aqueous solution
Substance.
Embodiment 5
One kind (Zr, Hf) B2The preparation method of ceramic powder.Preparation method described in the present embodiment is:
By reducing agent: contain (Zr, Hf) compound: boron source: the mass ratio of alkali metal-containing compound fused salt is 1.0: (2.0~
3.5): (1.0~2.5): (4.5~10.0) by the reducing agent, described containing (Zr, Hf) compound, the boron source and described contain
Alkali metal compound fused salt is uniformly mixed, dry, 4.5~7h is heat-treated under the conditions of protective atmosphere and 600~800 DEG C, so
It is dissolved, is washed under the conditions of 45~100 DEG C with aqueous slkali afterwards, it is dry, (Zr, Hf) B is made2Ceramic powder.
The reducing agent is aluminium powder.
(Zr, the Hf) compound that contains is (Zr, Hf) O2Powder.
The boron source is any one substance in boron cash, boric acid, sodium tetraborate, dipotassium tetraborate and lithium tetraborate.
The alkali metal-containing compound fused salt is sodium hydroxide, sodium metasilicate, sodium carbonate, potassium hydroxide, potassium silicate, carbonic acid
Any one substance in potassium, lithium hydroxide, lithium metasilicate, lithium carbonate and sodium aluminate.
The aqueous slkali is any one in sodium hydrate aqueous solution, potassium hydroxide aqueous solution and lithium hydroxide aqueous solution
Substance.
Embodiment 6
One kind (Zr, Hf) B2The preparation method of ceramic powder.Preparation method described in the present embodiment is:
By reducing agent: contain (Zr, Hf) compound: boron source: the mass ratio of alkali metal-containing compound fused salt is 1.0: (2.0~
3.5): (1.0~2.5): (4.5~10.0) by the reducing agent, described containing (Zr, Hf) compound, the boron source and described contain
Alkali metal compound fused salt is uniformly mixed, dry, 4.5~7h is heat-treated under the conditions of protective atmosphere and 600~800 DEG C, so
It is dissolved, is washed under the conditions of 45~100 DEG C with water afterwards, it is dry, (Zr, Hf) B is made2Ceramic powder.
The reducing agent is the mixture of silicon powder and aluminium powder.
(Zr, the Hf) compound that contains is (Zr, Hf) O2Powder.
The boron source is the mixing of any two substance in boron cash, boric acid, sodium tetraborate, dipotassium tetraborate and lithium tetraborate
Object.
The alkali metal-containing compound fused salt is sodium hydroxide, sodium metasilicate, sodium carbonate, potassium hydroxide, potassium silicate, carbonic acid
The mixture of any two substance in potassium, lithium hydroxide, lithium metasilicate, lithium carbonate and sodium aluminate.
Embodiment 7
One kind (Zr, Hf) B2The preparation method of ceramic powder.Preparation method described in the present embodiment is:
By reducing agent: contain (Zr, Hf) compound: boron source: the mass ratio of alkali metal-containing compound fused salt is 1.0: (2.0~
3.5): (1.0~2.5): (4.5~10.0) by the reducing agent, described containing (Zr, Hf) compound, the boron source and described contain
Alkali metal compound fused salt is uniformly mixed, dry, 4.5~7h is heat-treated under the conditions of protective atmosphere and 600~800 DEG C, so
It is dissolved, is washed under the conditions of 45~100 DEG C with water afterwards, it is dry, (Zr, Hf) B is made2Ceramic powder.
The reducing agent is silicon powder.
(Zr, the Hf) compound that contains is metal (Zr, Hf) powder.
The boron source is the mixing of any three kinds of substances in boron cash, boric acid, sodium tetraborate, dipotassium tetraborate and lithium tetraborate
Object.
The alkali metal-containing compound fused salt is sodium hydroxide, sodium metasilicate, sodium carbonate, potassium hydroxide, potassium silicate, carbonic acid
The mixture of any three kinds of substances of one of potassium, lithium hydroxide, lithium metasilicate, lithium carbonate and sodium aluminate.
Embodiment 8
One kind (Zr, Hf) B2The preparation method of ceramic powder.Preparation method described in the present embodiment is:
By reducing agent: contain (Zr, Hf) compound: boron source: the mass ratio of alkali metal-containing compound fused salt is 1.0: (2.0~
3.5): (1.0~2.5): (4.5~10.0) by the reducing agent, described containing (Zr, Hf) compound, the boron source and described contain
Alkali metal compound fused salt is uniformly mixed, dry, 4.5~7h is heat-treated under the conditions of protective atmosphere and 600~800 DEG C, so
It is dissolved, is washed under the conditions of 45~100 DEG C with aqueous slkali afterwards, it is dry, (Zr, Hf) B is made2Ceramic powder.
The reducing agent is aluminium powder.
(Zr, the Hf) compound that contains is (Zr, Hf) powder and (Zr, Hf) O2The mixture of powder.
The boron source is the above substance of any four in boron cash, boric acid, sodium tetraborate, dipotassium tetraborate and lithium tetraborate
Mixture.
The alkali metal-containing compound fused salt is sodium hydroxide, sodium metasilicate, sodium carbonate, potassium hydroxide, potassium silicate, carbonic acid
The mixture of the above substance of one of potassium, lithium hydroxide, lithium metasilicate, lithium carbonate and sodium aluminate any four.
The aqueous slkali is two kinds or more in sodium hydrate aqueous solution, potassium hydroxide aqueous solution and lithium hydroxide aqueous solution
The mixture of substance.
Embodiment 9
One kind (Zr, Hf) B2The preparation method of ceramic powder.Preparation method described in the present embodiment is:
By reducing agent: contain (Zr, Hf) compound: boron source: the mass ratio of alkali metal-containing compound fused salt is 1.0: (3.0~
4.5): (2.0~3.5): (9.0~14.0) by the reducing agent, described containing (Zr, Hf) compound, the boron source and described contain
Alkali metal compound fused salt is uniformly mixed, dry, and 2.5~5.0h is heat-treated under the conditions of protective atmosphere and 750~1000 DEG C,
Then it is dissolved, is washed under the conditions of room temperature~50 DEG C with water, it is dry, (Zr, Hf) B is made2Ceramic powder.
The reducing agent is the mixture of silicon powder and aluminium powder.
(Zr, the Hf) compound that contains is (Zr, Hf) O2Powder.
The boron source is any one substance in boron cash, boric acid, sodium tetraborate, dipotassium tetraborate and lithium tetraborate.
The alkali metal-containing compound fused salt is sodium hydroxide, sodium metasilicate, sodium carbonate, potassium hydroxide, potassium silicate, carbonic acid
Any one substance in potassium, lithium hydroxide, lithium metasilicate, lithium carbonate and sodium aluminate.
Embodiment 10
One kind (Zr, Hf) B2The preparation method of ceramic powder.Preparation method described in the present embodiment is:
By reducing agent: contain (Zr, Hf) compound: boron source: the mass ratio of alkali metal-containing compound fused salt is 1.0: (3.0~
4.5): (2.0~3.5): (9.0~14.0) by the reducing agent, described containing (Zr, Hf) compound, the boron source and described contain
Alkali metal compound fused salt is uniformly mixed, dry, and 2.5~5.0h is heat-treated under the conditions of protective atmosphere and 750~1000 DEG C,
Then it is dissolved, is washed under the conditions of room temperature~50 DEG C with aqueous slkali, it is dry, (Zr, Hf) B is made2Ceramic powder.
The reducing agent is silicon powder.
(Zr, the Hf) compound that contains is (Zr, Hf) O2Powder.
The boron source is the mixing of any two substance in boron cash, boric acid, sodium tetraborate, dipotassium tetraborate and lithium tetraborate
Object.
The alkali metal-containing compound fused salt is sodium hydroxide, sodium metasilicate, sodium carbonate, potassium hydroxide, potassium silicate, carbonic acid
The mixture of any two substance in potassium, lithium hydroxide, lithium metasilicate, lithium carbonate and sodium aluminate.
The aqueous slkali is any one in sodium hydrate aqueous solution, potassium hydroxide aqueous solution and lithium hydroxide aqueous solution
Substance.
Embodiment 11
One kind (Zr, Hf) B2The preparation method of ceramic powder.Preparation method described in the present embodiment is:
By reducing agent: contain (Zr, Hf) compound: boron source: the mass ratio of alkali metal-containing compound fused salt is 1.0: (3.0~
4.5): (2.0~3.5): (9.0~14.0) by the reducing agent, described containing (Zr, Hf) compound, the boron source and described contain
Alkali metal compound fused salt is uniformly mixed, dry, and 2.5~5.0h is heat-treated under the conditions of protective atmosphere and 750~1000 DEG C,
Then it is dissolved, is washed under the conditions of room temperature~50 DEG C with water, it is dry, (Zr, Hf) B is made2Ceramic powder.
The reducing agent is aluminium powder.
(Zr, the Hf) compound that contains is metal (Zr, Hf) powder.
The boron source is the mixing of any three kinds of substances in boron cash, boric acid, sodium tetraborate, dipotassium tetraborate and lithium tetraborate
Object.
The alkali metal-containing compound fused salt is sodium hydroxide, sodium metasilicate, sodium carbonate, potassium hydroxide, potassium silicate, carbonic acid
The mixture of any three kinds of substances in potassium, lithium hydroxide, lithium metasilicate, lithium carbonate and sodium aluminate.
Embodiment 12
One kind (Zr, Hf) B2The preparation method of ceramic powder.Preparation method described in the present embodiment is:
By reducing agent: contain (Zr, Hf) compound: boron source: the mass ratio of alkali metal-containing compound fused salt is 1.0: (3.0~
4.5): (2.0~3.5): (9.0~14.0) by the reducing agent, described containing (Zr, Hf) compound, the boron source and described contain
Alkali metal compound fused salt is uniformly mixed, dry, and 2.5~5.0h is heat-treated under the conditions of protective atmosphere and 750~1000 DEG C,
Then it is dissolved, is washed under the conditions of room temperature~50 DEG C with aqueous slkali, it is dry, (Zr, Hf) B is made2Ceramic powder.
The reducing agent is the mixture of silicon powder and aluminium powder.
(Zr, the Hf) compound that contains is (Zr, Hf) powder and (Zr, Hf) O2The mixture of powder.
The boron source is the above substance of any four in boron cash, boric acid, sodium tetraborate, dipotassium tetraborate and lithium tetraborate
Mixture.
The alkali metal-containing compound fused salt is sodium hydroxide, sodium metasilicate, sodium carbonate, potassium hydroxide, potassium silicate, carbonic acid
The mixture of the above substance of one of potassium, lithium hydroxide, lithium metasilicate, lithium carbonate and sodium aluminate any four.
The aqueous slkali is two kinds or more in sodium hydrate aqueous solution, potassium hydroxide aqueous solution and lithium hydroxide aqueous solution
The mixture of substance.
Embodiment 13
One kind (Zr, Hf) B2The preparation method of ceramic powder.Preparation method described in the present embodiment is:
By reducing agent: contain (Zr, Hf) compound: boron source: the mass ratio of alkali metal-containing compound fused salt is 1.0: (4.0~
5.0): (3.0~4.0): (13.0~18.0), by the reducing agent, described containing (Zr, Hf) compound, the boron source and described
Alkali metal-containing compound fused salt is uniformly mixed, dry, it is heat-treated 0.5 under the conditions of protective atmosphere and 850~1200 DEG C~
Then 3.0h is dissolved under the conditions of 195~250 DEG C with water, wash, dry, and (Zr, Hf) B is made2Ceramic powder.
The reducing agent is silicon powder.
(Zr, the Hf) compound that contains is (Zr, Hf) O2Powder.
The boron source is any one substance in boron cash, boric acid, sodium tetraborate, dipotassium tetraborate and lithium tetraborate.
The alkali metal-containing compound fused salt is sodium hydroxide, sodium metasilicate, sodium carbonate, potassium hydroxide, potassium silicate, carbonic acid
Any one substance of one of potassium, lithium hydroxide, lithium metasilicate, lithium carbonate and sodium aluminate.
Embodiment 14
One kind (Zr, Hf) B2The preparation method of ceramic powder.Preparation method described in the present embodiment is:
By reducing agent: contain (Zr, Hf) compound: boron source: the mass ratio of alkali metal-containing compound fused salt is 1.0: (4.0~
5.0): (3.0~4.0): (13.0~18.0), by the reducing agent, described containing (Zr, Hf) compound, the boron source and described
Alkali metal-containing compound fused salt is uniformly mixed, dry, it is heat-treated 0.5 under the conditions of protective atmosphere and 850~1200 DEG C~
Then 3.0h is dissolved under the conditions of 195~250 DEG C with aqueous slkali, wash, dry, and (Zr, Hf) B is made2Ceramic powder.
The reducing agent is aluminium powder.
(Zr, the Hf) compound that contains is (Zr, Hf) O2Powder.
The boron source is the mixing of any two substance in boron cash, boric acid, sodium tetraborate, dipotassium tetraborate and lithium tetraborate
Object.
The alkali metal-containing compound fused salt is sodium hydroxide, sodium metasilicate, sodium carbonate, potassium hydroxide, potassium silicate, carbonic acid
The mixture of any two substance of one of potassium, lithium hydroxide, lithium metasilicate, lithium carbonate and sodium aluminate.
The aqueous slkali is any one in sodium hydrate aqueous solution, potassium hydroxide aqueous solution and lithium hydroxide aqueous solution
Substance.
Embodiment 15
One kind (Zr, Hf) B2The preparation method of ceramic powder.Preparation method described in the present embodiment is:
By reducing agent: contain (Zr, Hf) compound: boron source: the mass ratio of alkali metal-containing compound fused salt is 1.0: (4.0~
5.0): (3.0~4.0): (13.0~18.0), by the reducing agent, described containing (Zr, Hf) compound, the boron source and described
Alkali metal-containing compound fused salt is uniformly mixed, dry, it is heat-treated 0.5 under the conditions of protective atmosphere and 850~1200 DEG C~
Then 3.0h is dissolved under the conditions of 195~250 DEG C with water, wash, dry, and (Zr, Hf) B is made2Ceramic powder.
The reducing agent is the mixture of silicon powder and aluminium powder.
(Zr, the Hf) compound that contains is metal (Zr, Hf) powder.
The boron source is the mixing of any three kinds of substances in boron cash, boric acid, sodium tetraborate, dipotassium tetraborate and lithium tetraborate
Object.
The alkali metal-containing compound fused salt is sodium hydroxide, sodium metasilicate, sodium carbonate, potassium hydroxide, potassium silicate, carbonic acid
The mixture of any three kinds of substances of one of potassium, lithium hydroxide, lithium metasilicate, lithium carbonate and sodium aluminate.
Embodiment 16
One kind (Zr, Hf) B2The preparation method of ceramic powder.Preparation method described in the present embodiment is:
By reducing agent: contain (Zr, Hf) compound: boron source: the mass ratio of alkali metal-containing compound fused salt is 1.0: (4.0~
5.0): (3.0~4.0): (13.0~18.0), by the reducing agent, described containing (Zr, Hf) compound, the boron source and described
Alkali metal-containing compound fused salt is uniformly mixed, dry, it is heat-treated 0.5 under the conditions of protective atmosphere and 850~1200 DEG C~
Then 3.0h is dissolved under the conditions of 195~250 DEG C with aqueous slkali, wash, dry, and (Zr, Hf) B is made2Ceramic powder.
The reducing agent is silicon powder.
(Zr, the Hf) compound that contains is (Zr, Hf) powder and (Zr, Hf) O2The mixture of powder.The boron source is boron cash, boron
The mixture of the above substance of any four in acid, sodium tetraborate, dipotassium tetraborate and lithium tetraborate.
The alkali metal-containing compound fused salt is sodium hydroxide, sodium metasilicate, sodium carbonate, potassium hydroxide, potassium silicate, carbonic acid
The mixture of the above substance of any four in potassium, lithium hydroxide, lithium metasilicate, lithium carbonate and sodium aluminate.
The aqueous slkali is two kinds or more in sodium hydrate aqueous solution, potassium hydroxide aqueous solution and lithium hydroxide aqueous solution
The mixture of substance.
Present embodiment has following good effect compared with prior art:
1, present embodiment introduces alkali metal-containing compound fused salt, alkali metal-containing compound fused salt in the reaction system
Presence, can form liquid phase at a lower temperature, strengthen mass transport process, improve the dynamic conditions of chemical reaction, improve also
Former reaction efficiency.After introducing alkali metal-containing compound fused salt, reaction carries out in the liquid phase, and reaction condition is mild, generation (Zr,
Hf)B2Ceramic powder has the characteristics that partial size is small, narrow particle size distribution.
Fig. 1 is (Zr, Hf) B made from embodiment 22The XRD spectrum of ceramic powder, it will be seen from figure 1 that (Zr, Hf) B2Pottery
Other miscellaneous phases are had no in porcelain powder, calculate average grain size is about 45nm；Fig. 2 is (Zr, Hf) B shown in Fig. 12Ceramic powder
SEM photograph, figure it is seen that (Zr, Hf) B obtained2Diameter of particle is uniform, is loose aggregate.Fig. 3 is embodiment
(Zr, Hf) B made from 132The XRD spectrum of ceramic powder, from figure 3, it can be seen that (Zr, Hf) B2Have no other miscellaneous in ceramic powder
Phase, calculate average grain size is about 62nm.
2, the present invention boron-containing compounds such as boric acid, sodium tetraborate, dipotassium tetraborate, lithium tetraborate can be used to make in addition to boric anhydride
For boron source, raw material sources are widened, production cost is low.
3, the alkali metal-containing compound fused salt that the present invention uses can participate in chemically reacting, and improve the thermodynamics item of chemical reaction
Part promotes the progress of reduction reaction, improves yield and the rate of recovery.Product after heat treatment is directly washed or alkali cleaning, simple process,
Byproduct recoverable avoids traditional acid cleaning process and causes the drawbacks of seriously polluting to environment, it is environmental-friendly, be easy to industry
Metaplasia produces.
Claims (5)
1. one kind (Zr, Hf) B2The preparation method of ceramic powder, it is characterised in that the preparation method is:
By reducing agent: contain (Zr, Hf) compound: boron source: the mass ratio of alkali metal-containing compound fused salt is 1.0: (1.0~5.0):
(0.7~4.0): (0.2~18.0), by the reducing agent, it is described containing (Zr, Hf) compound, the boron source and it is described containing alkali gold
Belong to compound fused salt to be uniformly mixed, it is dry, it is heat-treated 0.5~8h under the conditions of protective atmosphere and 600~1300 DEG C, then uses
Water or aqueous slkali dissolve under the conditions of room temperature~250 DEG C, wash, dry, and (Zr, Hf) B is made2Ceramic powder；
The reducing agent be silicon powder or be aluminium powder or be silicon powder and aluminium powder mixture；
(Zr, the Hf) compound that contains is metal (Zr, Hf) powder and (Zr, Hf) O2One or more of powder；
The boron source is one or more of boron cash, boric acid, sodium tetraborate, dipotassium tetraborate and lithium tetraborate；
The alkali metal-containing compound fused salt is sodium hydroxide, sodium metasilicate, sodium carbonate, potassium hydroxide, potassium silicate, potassium carbonate, hydrogen
One or more of lithia, lithium metasilicate, lithium carbonate and sodium aluminate.
2. (Zr, Hf) B according to claim 12The preparation method of ceramic powder is characterized in that the aqueous slkali is hydroxide
One or more of sodium water solution, potassium hydroxide aqueous solution and lithium hydroxide aqueous solution.
3. (Zr, Hf) B according to claim 12The preparation method of ceramic powder, it is characterised in that SiO in the sodium metasilicate2
With Na2Molar ratio≤1 of O.
4. (Zr, Hf) B according to claim 12The preparation method of ceramic powder, it is characterised in that SiO in the potassium silicate2
With K2Molar ratio≤1 of O.
5. (Zr, Hf) B according to claim 12The preparation method of ceramic powder, it is characterised in that SiO in the lithium metasilicate2
With Li2Molar ratio≤1 of O.
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| PCT/CN2019/105343 WO2020073767A1 (en) | 2018-10-11 | 2019-09-11 | Preparation method for tib 2 or (zr, hf) b 2 ceramic powder |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110318254A (en) * | 2019-08-11 | 2019-10-11 | 西南石油大学 | A kind of carbon fiber surface HfB2The preparation method of coating |
| WO2020073767A1 (en) * | 2018-10-11 | 2020-04-16 | 武汉科技大学 | Preparation method for tib 2 or (zr, hf) b 2 ceramic powder |
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| US4929417A (en) * | 1989-04-21 | 1990-05-29 | Agency Of Industrial Science And Technology | Method of manufacture metal diboride ceramics |
| CN103848619A (en) * | 2012-12-03 | 2014-06-11 | 南京理工大学 | Micro-nano intragranular multiphase granule and thermal explosion reaction synthetic method thereof |
| CN106631033A (en) * | 2016-12-27 | 2017-05-10 | 北京有色金属研究总院 | Method for preparing ZrB2 powder |
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| US4929417A (en) * | 1989-04-21 | 1990-05-29 | Agency Of Industrial Science And Technology | Method of manufacture metal diboride ceramics |
| CN103848619A (en) * | 2012-12-03 | 2014-06-11 | 南京理工大学 | Micro-nano intragranular multiphase granule and thermal explosion reaction synthetic method thereof |
| CN106631033A (en) * | 2016-12-27 | 2017-05-10 | 北京有色金属研究总院 | Method for preparing ZrB2 powder |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| WO2020073767A1 (en) * | 2018-10-11 | 2020-04-16 | 武汉科技大学 | Preparation method for tib 2 or (zr, hf) b 2 ceramic powder |
| CN110318254A (en) * | 2019-08-11 | 2019-10-11 | 西南石油大学 | A kind of carbon fiber surface HfB2The preparation method of coating |
| CN110318254B (en) * | 2019-08-11 | 2021-12-03 | 西南石油大学 | HfB on surface of carbon fiber2Method for producing a coating |
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| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20190122 |
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| RJ01 | Rejection of invention patent application after publication |