CN101774580B - Method for purifying zirconium carbide powder - Google Patents
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Abstract
The invention relates to a method for purifying refractory compound powder, in particular to a method for purifying zirconium carbide powder, which is characterized in that the method includes the following steps: 1)selecting 85-99% of ZrC power and 1-15% of Mg powder by weight percent for later use; 2) mixing the ZrC power and the Mg power to get power mixture, putting the power mixture into a mold, putting the mold in a thermal treatment furnace for heat treatment, and filling argon to be used as protective atmosphere for heat treatment; 3)grinding the products obtained from the heat treatment process, screening to get powder with grain size smaller than 0.5mm, pickling the powder in hydrochloric acid at concentration of 0.5-2.0mol/L for 1-12h under 20-80 DEG C, filtering and drying the product. In this way, high-purity zirconium carbide powder can be obtained. The method is simple in process and low in cost and the zirconium carbide powder is high in purity after being purified through the method.
Description
Technical field
The present invention relates to a kind of method of purification of infusible compound powder, be specifically related to a kind of method of purifying zirconium carbide powder.
Background technology
Zirconium carbide is a kind of material more common in the carbide material, also is the research focus of non-oxide ceramic material in recent years, can also be the raw material of production atomic level zirc sponge as the additive of high grade refractory.Because its hot strength and hardness are high, thermal neutron absorption cross section is little, radiation resistance good, is selected as the novel material on coated nuclear fuel particle blocking layer.And nano-zirconium carbide has the efficient absorption visible light, the characteristic of reflected infrared; After its absorbs the short wavelength's energy account in the sunshine below 95% the 2 μ m; Through thermal cross over, can the energy be stored in the material, it also has the characteristic that reflection surpasses 2 μ m IR wavelengths.And the infrared wave that human body produces is about about 10 μ m, can outwards not distribute.This explanation zirconium carbide has the characteristic of ideal heat absorption, accumulation of heat.Zirconium carbide ceramics belongs to superhard material; Chemicalstability is good; Having good high temperature resistant, corrosion-resistant, wear resisting property, is the good high-temperature structured material, superhard tool material and surface protecting material; It also has good thermal conductivity simultaneously, has the potential using value in directions such as cutter material, armour material, build-up wear-resistant welding rods.
Zirconium carbide is a kind of non-stoichiometric carbide that transition element Zr and C form, and in carbon-zirconium system, has the nonstoichiometry phenomenon of wide range, i.e. ZrC
x(0.5≤x≤1); This is because the NaCl type crystal structure is a kind of metastable state structure; In the ZrC crystal; Though Zr atom and C atom all are on the face-centred cubic lattice, the room only is present in the position at C atom place, therefore in the carbide of this non-stoichiometric, also has the existence of uncombined carbon.Research shows that the ZrC that measures ratio fully is non-existent, and very easily oxidation of ZrC, and its oxidizing temperature is about 300 ℃.Thereby the position of O atom instead C atom forms Zr (C
xO
y) compound.
The traditional synthesis of zirconium carbide ceramics powder is: carbothermic method, sol-gel method, low temperature synthesis method, combustion synthesis method etc.Commercially available zirconium carbide powder is by the carbothermic method synthetic mostly.Though can reach tens to the hundreds of nanometer by these technology synthetic zirconium carbide powder particle diameters, because the influence of factors such as technology and raw material, and very easily oxidation of zirconium carbide, so the not high problem of ubiquity purity.
Reference
[1]Yan，Y.J.Huang，Z.G.Liu，X.J.Jiang，D.L.Journal?of?Sol-Gel?Scienceand?Technology，2007，44，81-85.
[2]Sun?shouren.hand?book?of?Material?for?Nuclear?reactor[M].Beijing：AtomicEnergy?Press，1987：26.
[3]Ogawa?T?et?al.Journal?of?Rare?metal?Material?and?Engineering，2000，29(2)：101.
[4]M.D.Sack?et?al.，Journal?of?Materials?and?Science.2004，39，6057.
[5]Norton?et?al.，US?Patent#N63-18389，Advanced?Materials?Research?Corp.
[6]D.Gosset，M.Dolle，Nucl.Instr.And?Meth.In?Phys.Res.B，2008，266，2801-2805.
[7]S.Shimada.T.Ishii，J.Am.Ceram.Soc，1990，73，2804-808.
Summary of the invention
The object of the present invention is to provide a kind of method of purifying zirconium carbide powder, this method technology is simple, cost is low, and the zirconium carbide powder purity that obtains is high.
To achieve these goals, the technical scheme that the present invention taked is: a kind of method of purifying zirconium carbide powder, and adopt reduction heat to handle, it is characterized in that it comprises the steps:
1) by the shared weight percentage of each raw material be: the ZrC powder: 85～99%, Mg powder: 1～15%, choose ZrC powder and Mg powder, subsequent use;
2) with ZrC powder and Mg powder uniform mixing, obtain mixed powder; Mixed powder put into mould, place in the heat treatment furnace, and applying argon gas is as protective atmosphere (air pressure of argon gas is 0.02Mpa), adopt one of following two kinds heat-treating:
1. said heat treatment furnace is a tube furnace, and thermal treatment temp in tube furnace and time are: temperature is 1300～1500 ℃, and soaking time is 1h, obtains the thermal treatment product;
2. said heat treatment furnace is discharge plasma sintering stove (SPS), and thermal treatment temp in the discharge plasma sintering stove and time are: temperature is 1300～1700 ℃, and soaking time is 5～15min, obtains the thermal treatment product;
3) with the thermal treatment product after grinding; Sieve and obtain the powder of particle diameter less than 0.5mm; With powder place concentration be the hydrochloric acid of 0.5～2.0mol/L in 20～80 ℃ of pickling 1～12 hour, obtained product through filter, oven dry, obtain the zirconium carbide powder of high purity (mass content >=98.0%).
The described ZrC powder of step 1) is commercially available ZrC powder or laboratory synthetic ZrC powder, and the particle diameter of ZrC powder is 80nm～5 μ m, and the mass content of oxygen is 3%～5% in the ZrC powder, other impurity mass content≤4% (being mainly elements such as Fe, Cl, Mg) in the ZrC powder.
The particle diameter of the described Mg powder of step 1) is 74 μ m.
The shared weight percentage of described each raw material of step 1) is: the ZrC powder: 95%, and the Mg powder: 5%, wherein the particle diameter of ZrC powder is 1 μ m.
The shared weight percentage of described each raw material of step 1) is: the ZrC powder: 90%, and the Mg powder: 10%, wherein the particle diameter of ZrC powder is 80nm.
The shared weight percentage of described each raw material of step 1) is: the ZrC powder: 95%, and the Mg powder: 5%, wherein the particle diameter of ZrC powder is 200nm～300nm.
Step 2) describedly with ZrC powder and Mg powder uniform mixing be: with ZrC powder and Mg powder under vacuum condition dry 10～20 hours, with ZrC powder and Mg powder mechanical ball milling mixing 1～3h, ball-to-powder weight ratio was 3: 1 again.
The present invention has following beneficial effect:
1, the property of zirconium carbide makes it obtain widespread production and application; Do not limited its application again but purity is high; The present invention adopts subsequent heat treatment that the synthetic zirconium carbide of commercially available zirconium carbide or laboratory is carried out purification processes, and technology is simple, and cost is lower; But product purity improves a lot, for its widespread use provides guarantee.
2, the present invention adopts common tube furnace as heat treatment furnace, has certain ubiquity, is applicable to laboratory and industrial production.Technology is simple, and cost is low, and is higher through the product purity of purifying.
3, the present invention adopts the discharge plasma sintering stove as heat treatment furnace; Mainly utilize the electric field clear powder resin particle surface oxide compound of applying pulse strong current formation and the gas of absorption, scavenging material, activating powder surface; Help the removal of impurity such as oxygen in the zirconium carbide powder, thereby improve purity.
Description of drawings
Fig. 1 is the SEM figure of embodiment 2 gained zirconium carbide powders.
Fig. 2 is the XRD figure of embodiment 2 gained zirconium carbide powders.
Fig. 3 is the SEM figure of embodiment 3 gained zirconium carbide powders.
Fig. 4 is the SEM figure of embodiment 5 gained zirconium carbide powders.
Embodiment
In order to understand the present invention better, further illustrate content of the present invention below in conjunction with instance, but content of the present invention not only is confined to following embodiment.
Embodiment 1:
A kind of method of purifying zirconium carbide powder adopts reduction heat to handle, and it comprises the steps:
1) the raw material powder particle diameter is respectively: ZrC powder 1 μ m, Mg powder 74 μ m; The ZrC powder is commercially available ZrC powder, knows that through the analysis of nitrogen oxygen the massfraction of oxygen in the ZrC powder is 3.8%, and other major impurity content are 2.06% (Fe is 0.97%, and Cl is 1.09%); By the shared weight percentage of each raw material be: the ZrC powder: 95%, the Mg powder: 5%, choose ZrC powder and Mg powder, subsequent use;
2) with ZrC powder and Mg powder under vacuum condition dry 10 hours, with ZrC powder and Mg powder mechanical ball milling mixing 2h, ball-to-powder weight ratio was 3: 1, obtains mixed powder again;
Mixed powder is packed in the mould, place tube furnace, applying argon gas is as protective atmosphere, and air pressure is 0.02Mpa; Treatment temp is 1300 ℃, and soaking time is 1h, obtains the thermal treatment product;
3) with the thermal treatment product after grinding, sieving obtains the powder of particle diameter less than 0.5mm, with powder place concentration be the hydrochloric acid of 2.0mol/L in 60 ℃ of pickling 12 hours, obtained product through filter, oven dry, obtain highly purified zirconium carbide powder.
The composition of measuring resultant highly purified zirconium carbide powder shows: obtain that ZrC content is 98.0% in the highly purified zirconium carbide powder, particle diameter is 1 μ m, does not have and obviously grows up.The impurity mass content is seen table 1 in the resultant highly purified zirconium carbide powder.
Embodiment 2:
A kind of method of purifying zirconium carbide powder adopts reduction heat to handle, and it comprises the steps:
1) the raw material powder particle diameter is respectively: ZrC powder 80nm, Mg powder 74 μ m; The ZrC powder is commercially available ZrC powder, knows that through the analysis of nitrogen oxygen the mass content of oxygen in the ZrC powder is 5%, and other major impurity content are 2.37% (Fe is 0.24%, and Cl is 2.13%); By the shared weight percentage of each raw material be: the ZrC powder: Mg powder 90%: 10%, choose ZrC powder and Mg powder, subsequent use;
2) with ZrC powder and Mg powder under vacuum condition dry 10 hours, with ZrC powder and Mg powder mechanical ball milling mixing 3h, ball-to-powder weight ratio was 3: 1, obtains mixed powder again; Mixed powder is put into mould, place tube furnace, applying argon gas is as protective atmosphere, and air pressure is 0.02Mpa, and treatment temp is 1500 ℃, and soaking time is 1h, obtains the thermal treatment product;
3) with the thermal treatment product after grinding, sieving obtains the powder of particle diameter less than 0.5mm, with powder place concentration be the hydrochloric acid of 2.0mol/L in 60 ℃ of pickling 12 hours, obtained product through filter, oven dry, obtain highly purified zirconium carbide powder.
The composition of measuring resultant highly purified zirconium carbide powder shows: ZrC content is 98.7% in the highly purified zirconium carbide powder that obtains, and particle diameter is 100nm.See Fig. 1, Fig. 2.From the SEM photo of Fig. 1 powder, can find out; The particle diameter of the zirconium carbide powder that makes is about 100nm; See that from the XRD figure of Fig. 2 powder the diffraction peak of the powder of gained corresponds to the diffraction peak of zirconium carbide, explain that the zirconium carbide powder purity that obtains is high, particle diameter is tiny.The impurity mass content is seen table 1 in the resultant highly purified zirconium carbide powder.
Embodiment 3:
A kind of method of purifying zirconium carbide powder adopts reduction heat to handle, and it comprises the steps:
1) the raw material powder particle diameter is respectively: ZrC powder 200～300nm, Mg powder 74 μ m; The ZrC powder is a laboratory synthetic ZrC powder, and the mass content of oxygen is 3.02% in the ZrC powder, and other major impurity mass content are 0.48% (being mainly the Mg element); By the shared weight percentage of each raw material be: the ZrC powder: Mg powder 95%: 5%, choose ZrC powder and Mg powder, subsequent use;
2) with ZrC powder and Mg powder mechanical ball milling mixing 1h, ball-to-powder weight ratio is 3: 1, under vacuum condition dry 10 hours then, obtains mixed powder; Mixed powder is put into mould, place tube furnace, applying argon gas is as protective atmosphere, and air pressure is 0.02Mpa, and treatment temp is 1500 ℃, and soaking time is 1h, obtains the thermal treatment product;
3) with the thermal treatment product after grinding, sieving obtains the powder of particle diameter less than 0.5mm, with powder place concentration be the hydrochloric acid of 2.0mol/L in 60 ℃ of pickling 12 hours, obtained product through filter, oven dry, obtain highly purified zirconium carbide powder.
The composition of measuring resultant highly purified zirconium carbide powder shows: obtain that ZrC content is 99.0% in the highly purified zirconium carbide powder, particle diameter is 400nm.See Fig. 3, from figure, can find out that the particle diameter of the zirconium carbide powder that makes is about 400nm in the SEM photo of powder.The impurity mass content is seen table 1 in the resultant highly purified zirconium carbide powder.
Embodiment 4:
A kind of method of purifying zirconium carbide powder adopts reduction heat to handle, and it comprises the steps:
1) the raw material powder particle diameter is respectively: ZrC powder 200～300nm, Mg powder 74 μ m; The ZrC powder is a laboratory synthetic ZrC powder, and the mass content of oxygen is 3.02% in the ZrC powder, and other major impurity mass content are 0.48% (being mainly the Mg element); By the shared weight percentage of each raw material be: the ZrC powder: Mg powder 95%: 5%, choose ZrC powder and Mg powder, subsequent use;
2) with ZrC powder and Mg powder under vacuum condition dry 20 hours, with ZrC powder and Mg powder mechanical ball milling mixing 3h, ball-to-powder weight ratio was 3: 1, obtains mixed powder again; Mixed powder is put into mould, place the discharge plasma sintering stove, applying argon gas is as protective atmosphere, and treatment temp is 1500 ℃, and soaking time is 15min, obtains the thermal treatment product;
3) with the thermal treatment product after grinding, sieving obtains the powder of particle diameter less than 0.5mm, with powder place concentration be the hydrochloric acid of 1.0mol/L in 80 ℃ of pickling 10 hours, obtained product through filter, oven dry, obtain highly purified zirconium carbide powder.
Measure show to the composition of highly purified zirconium carbide powder: ZrC content is 99.2% in the product, and particle diameter is about 400nm.The impurity mass content is seen table 1 in the resultant highly purified zirconium carbide powder.
Embodiment 5:
A kind of method of purifying zirconium carbide powder adopts reduction heat to handle, and it comprises the steps:
1) the raw material powder particle diameter is respectively: ZrC powder 200～300nm, Mg powder 74 μ m; The ZrC powder is a laboratory synthetic ZrC powder, and the mass content of oxygen is 3.02% in the ZrC powder, and other major impurity mass content are 0.48% (being mainly the Mg element); By the shared weight percentage of each raw material be: the ZrC powder: Mg powder 95%: 5%, choose ZrC powder and Mg powder, subsequent use;
2) with ZrC powder and Mg powder under vacuum condition dry 10 hours, with ZrC powder and Mg powder mechanical ball milling mixing 2h, ball-to-powder weight ratio was 3: 1, obtains mixed powder again; Mixed powder is put into mould, place the discharge plasma sintering stove, applying argon gas is as protective atmosphere, and the air pressure of argon gas is 0.02Mpa, and treatment temp is 1700 ℃, and soaking time is 15min, obtains the thermal treatment product;
3) with the thermal treatment product after grinding, sieving obtains the powder of particle diameter less than 0.5mm, with powder place concentration be the hydrochloric acid of 0.5mol/L in 20 ℃ of pickling 8 hours, obtained product through filter, oven dry, obtain highly purified zirconium carbide powder.
The composition of measuring resultant highly purified zirconium carbide powder shows: obtain that ZrC content is 99.6% in the highly purified zirconium carbide powder, particle diameter is 800nm.See Fig. 4, from figure, can find out that the particle diameter of the zirconium carbide powder that makes is about 800nm in the SEM photo of powder.The impurity mass content is seen table 1 in the resultant highly purified zirconium carbide powder.
Embodiment 6:
A kind of method of purifying zirconium carbide powder adopts reduction heat to handle, and it comprises the steps:
1) by the shared weight percentage of each raw material be: the ZrC powder: Mg powder 85%: 15%, choose ZrC powder and Mg powder, subsequent use; Described ZrC powder is commercially available ZrC powder, and the particle diameter of ZrC powder is 80nm, knows that through the analysis of nitrogen oxygen the mass content of oxygen in the ZrC powder is 5%, and other major impurity content are 2.37% (Fe is 0.24%, and Cl is 2.13%); The particle diameter of described Mg powder is 74 μ m.
2) with ZrC powder and Mg powder under vacuum condition dry 10 hours, with ZrC powder and Mg powder mechanical ball milling mixing 1h, ball-to-powder weight ratio was 3: 1, obtains mixed powder again; Mixed powder is put into mould; Place in the discharge plasma sintering stove (SPS), and applying argon gas is as protective atmosphere (air pressure of argon gas is 0.02Mpa) that thermal treatment temp in the discharge plasma sintering stove and time are: temperature is 1300 ℃; Soaking time is 5min, obtains the thermal treatment product;
3) with the thermal treatment product after grinding, sieving obtains the powder of particle diameter less than 0.5mm, with powder place concentration be the hydrochloric acid of 0.5mol/L in 20 ℃ of pickling 1 hour, obtained product through filter, oven dry, obtain zirconium carbide powder (purity is 98.45%).
The impurity mass content is seen table 1 in the resultant highly purified zirconium carbide powder.
Embodiment 7:
A kind of method of purifying zirconium carbide powder adopts reduction heat to handle, and it comprises the steps:
1) by the shared weight percentage of each raw material be: the ZrC powder: Mg powder 99%: 1%, choose ZrC powder and Mg powder, subsequent use; Described ZrC powder is commercially available ZrC powder, and the particle diameter of ZrC powder is 5 μ m, and the mass content of oxygen is 3% in the ZrC powder, and other impurity mass content are 1% (being mainly the Fe element) in the ZrC powder; The particle diameter of described Mg powder is 74 μ m.
2) with ZrC powder and Mg powder under vacuum condition dry 20 hours, with ZrC powder and Mg powder mechanical ball milling mixing 3h, ball-to-powder weight ratio was 3: 1, obtains mixed powder again; Mixed powder is put into mould; Place in the discharge plasma sintering stove (SPS), and applying argon gas is as protective atmosphere (air pressure of argon gas is 0.02Mpa) that thermal treatment temp in the discharge plasma sintering stove and time are: temperature is 1700 ℃; Soaking time is 15min, obtains the thermal treatment product;
3) with the thermal treatment product after grinding, sieving obtains the powder of particle diameter less than 0.5mm, with powder place concentration be the hydrochloric acid of 2.0mol/L in 80 ℃ of pickling 10 hours, obtained product through filter, oven dry, obtain the zirconium carbide powder of high purity (purity is 98.8%).
The impurity mass content is seen table 1 in the resultant highly purified zirconium carbide powder.
Table 1 impurity mass content
| Embodiment | 1 | 2 | 3 | 4 | 5 | 6 | 7 |
| The mass content of oxygen (%) | 1.75 | 1.02 | 0.85 | 0.68 | 0.30 | 1.20 | 0.90 |
| The mass content of other impurity (%) | 0.25 | 0.28 | 0.15 | 0.12 | 0.10 | 0.35 | 0.30 |
Claims (4)
1. the method for a purifying zirconium carbide powder is characterized in that it comprises the steps:
1) by the shared weight percentage of each raw material be: the ZrC powder: 85～99%, Mg powder: 1～15%, choose ZrC powder and Mg powder, subsequent use;
2) with ZrC powder and Mg powder uniform mixing, obtain mixed powder; Mixed powder put into mould, place in the heat treatment furnace, and applying argon gas is as protective atmosphere, adopt one of following two kinds heat-treating:
1. said heat treatment furnace is a tube furnace, and thermal treatment temp in tube furnace and time are: temperature is 1300～1500 ℃, and soaking time is 1h, obtains the thermal treatment product;
2. said heat treatment furnace is the discharge plasma sintering stove, and thermal treatment temp in the discharge plasma sintering stove and time are: temperature is 1300～1700 ℃, and soaking time is 5～15min, obtains the thermal treatment product;
3) with the thermal treatment product after grinding, sieving obtains the powder of particle diameter less than 0.5mm, with powder place concentration be the hydrochloric acid of 0.5～2.0mol/L in 20～80 ℃ of pickling 1～12 hour, obtained product through filter, oven dry, obtain highly purified zirconium carbide powder;
The described ZrC powder of step 1) is commercially available ZrC powder or laboratory synthetic ZrC powder, and the particle diameter of ZrC powder is 80nm～5 μ m, and the mass content of oxygen is 3%～5% in the ZrC powder, other impurity mass content≤4% in the ZrC powder;
The particle diameter of the described Mg powder of step 1) is 74 μ m;
Step 2) describedly with ZrC powder and Mg powder uniform mixing be: with ZrC powder and Mg powder under vacuum condition dry 10～20 hours, with ZrC powder and Mg powder mechanical ball milling mixing 1～3h, ball-to-powder weight ratio was 3: 1 again.
2. the method for a kind of purifying zirconium carbide powder according to claim 1, it is characterized in that: the shared weight percentage of described each raw material of step 1) is: the ZrC powder: 95%, the Mg powder: 5%, wherein the particle diameter of ZrC powder is 1 μ m.
3. the method for a kind of purifying zirconium carbide powder according to claim 1, it is characterized in that: the shared weight percentage of described each raw material of step 1) is: the ZrC powder: 90%, the Mg powder: 10%, wherein the particle diameter of ZrC powder is 80nm.
4. the method for a kind of purifying zirconium carbide powder according to claim 1, it is characterized in that: the shared weight percentage of described each raw material of step 1) is: the ZrC powder: 95%, the Mg powder: 5%, wherein the particle diameter of ZrC powder is 200nm～300nm.
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| Title |
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| 付志强等.化学气相沉积法制备ZrC涂层的热力学分析.《原子能科学技术》.2007,第41卷(第3期),第297-300页. * |
| 陈磊等.ZrCl4蒸汽沉积法制备高温气冷堆包覆燃料颗粒ZrC涂层.《原子能科学技术》.2009,第43卷(第11期),第1017-1020页. * |
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