阅读说明：本技术 一种纤维增塑性吸气粉末的轧制方法 (Rolling method of fiber plasticizing air suction powder ) 是由 鲁涛 于 2019-12-27 设计创作，主要内容包括：本发明公布了一种纤维增塑性吸气粉末的轧制方法,所述方法包括如下步骤：将吸气合金中的原料按一定比例进行配制,通过熔炼的方法制备成合金,然后对合金在保护气氛下进行破碎和球磨,获得325目~80目的吸气合金粉末；用上述吸气合金粉末与与0.01~2%(质量分数)硬脂酸混合均匀形成合金粉末；用上述合金粉末与0.1~70%wt%钛及钛合金纤维均匀混合形成合金混合物；将上述合金混合物在室温下通过轧机进行粉末轧制形成轧制板；在真空度为3~6×10<Sup>-3 </Sup>Pa的真空环境下,对轧制板进行真空烧结,即可得到纤维增塑性吸气轧制板。本发明工艺流程短、节能、成本较低、压坯或产品成分精确可控、成材率较高。(The invention discloses a rolling method of fiber plasticizing air suction powder, which comprises the following steps: preparing raw materials in the air suction alloy according to a certain proportion, preparing the air suction alloy into an alloy by a smelting method, and then crushing and ball-milling the alloy in a protective atmosphere to obtain 325-80 mesh air suction alloy powder; the getter alloy powder is mixed with 0.01-2 wt%Fraction) stearic acid is mixed evenly to form alloy powder; uniformly mixing the alloy powder with 0.1-70 wt% of titanium and titanium alloy fibers to form an alloy mixture; performing powder rolling on the alloy mixture at room temperature through a rolling mill to form a rolled plate; under a vacuum degree of 3 to 6 x 10 ‑3 And (3) carrying out vacuum sintering on the rolled plate under the vacuum environment of Pa to obtain the fiber plasticizing suction rolled plate. The invention has the advantages of short process flow, energy saving, lower cost, accurate and controllable pressed blank or product components and higher yield.)

1. A rolling method of fiber plasticizing gas absorption powder is characterized in that the rolling method of fiber plasticizing gas absorption powder is carried out according to the following steps:

1) preparing raw materials in the air suction alloy according to a certain proportion, preparing the air suction alloy into an alloy by a smelting method, and then crushing and ball-milling the alloy in a protective atmosphere to obtain 325-80 mesh air suction alloy powder;

2) mixing the getter alloy powder with 0.01-2% (mass fraction) of stearic acid uniformly to form alloy powder;

3) uniformly mixing the alloy powder with 0.1-70 wt% of titanium and titanium alloy fibers to form an alloy mixture;

4) performing powder rolling on the alloy mixture at room temperature through a rolling mill to form a rolled plate;

5) under a vacuum degree of 3 to 6 x 10^-3And (3) carrying out vacuum sintering on the rolled plate under the vacuum environment of Pa to obtain the fiber plasticizing suction rolled plate.

2. The rolling method of fiber plasticizing getter powder according to claim 1, characterized in that: the kinds of the alloy include:

a) Zr-Al alloy, Zr-Al-RE alloy, Zr-Al-TE-RE alloy, wherein TE comprises transition group elements of Ti, Fe, Co, Ni, Mn, Pd, Ru, Pt, V, Cr, Nb, Mo, Tc, Rh, Hf, Ta, W, Re, Os and Ir;

b) Zr-C alloy, Zr-C-RE alloy, Zr-C-TE-RE alloy, wherein TE comprises transition group elements of Ti, Fe, Co, Ni, Mn, Pd, Ru, Pt, V, Cr, Nb, Mo, Tc, Rh, Hf, Ta, W, Re, Os and Ir;

c) Zr-V-Fe alloy, Zr-V-Fe-RE alloy, Zr-V-Fe-TE alloy, Zr-V-Fe-RE-TE alloy, wherein TE comprises transition elements of Ti, Co, Ni, Mn, Pd, Ru, Pt, Cr, Nb, Mo, Tc, Rh, Hf, Ta, W, Re, Os and Ir;

d) Zr-Co alloy, Zr-Co-RE alloy, Zr-Co-TE alloy, Zr-Co-RE-TE alloy, wherein TE comprises transition group elements of Ti, Fe, Ni, Mn, Pd, Ru, Pt, V, Cr, Nb, Mo, Tc, Rh, Hf, Ta, W, Re, Os and Ir;

e) Ti-Mo alloy, Ti-Mo-RE alloy, Ti-Mo-TE alloy, Ti-Mo-RE-TE alloy, wherein TE comprises transition group elements of Zr, Fe, Co, Ni, Mn, Pd, Ru, Pt, V, Cr, Nb, Tc, Rh, Hf, Ta, W, Re, Os and Ir;

f) Ti-Zr-V alloy, Ti-Zr-V-RE alloy, Ti-Zr-V-TE-RE alloy, wherein TE comprises transition group elements of Fe, Co, Ni, Mn, Pd, Ru, Pt, Cr, Nb, Mo, Tc, Rh, Hf, Ta, W, Re, Os and Ir;

g) Zr-Co-Re (rhenium) alloy, Zr-Co-Re-RE-TE alloy, wherein TE comprises transition elements of Ti, Fe, Co, Ni, Mn, Pd, Ru, Pt, V, Cr, Nb, Mo, Tc, Rh, Hf, Ta, W, Os and Ir.

3. The rolling method of fiber plasticizing getter powder according to claim 2, characterized in that: the RE comprises rare earth elements of Y, Sc, La, Ce, Pr, Nd, Pm, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb and Lu.

4. The rolling method of fiber plasticizing getter powder according to claim 1, characterized in that: the diameter of the titanium and titanium alloy fiber is 0.04-0.09 mm, and the length is 0.01-2 mm.

5. The rolling method of fiber plasticizing getter powder according to claim 1, characterized in that: the weight ratio of the titanium to the titanium alloy fiber is 0.1-70 wt%.

6. The rolling method of fiber plasticizing getter powder according to claim 1, characterized in that: the rolling pressure of the rolling mill is 10-120 kN, the rolling speed is 1-5 m/min, and the roll gap is 1-4 mm.

7. The rolling method of fiber plasticizing getter powder according to claim 1, characterized in that: the sintering process of the rolled plate is to keep the temperature at 1000-1200 ℃ for 0.2-2 h.

Technical Field

The invention relates to the field of aerospace industry, in particular to a rolling method of fiber plasticizing air suction powder.

Background

The powder rolling process is widely applied to the production of porous titanium alloy plates and porous air suction plates in the industries of filtration separation, energy environmental protection, fluid transportation, electrolytic hydrogen production and the like of the aerospace industry, the pharmaceutical industry, the petrochemical industry, the semiconductor industry and the like and an air suction and distribution system of the vacuum industry because of an efficient forming method.

In the powder rolling process, the porous getter material plates with different thicknesses and properties are prepared by controlling the feeding amount, the roll gap and the rolling speed in the metal powder rolling process. The technology can continuously and stably produce the metal plate-shaped filter element and the air suction element, and the plate-shaped filter element rolled by the technology has the characteristics of uniform thickness, uniform pore distribution, low production cost and the like. However, this technique has limited application to some brittle powders and the like, and therefore, some additives such as stearic acid or organic solvents need to be added to the powder to compensate.

Disclosure of Invention

The invention aims to provide a preparation method of an anti-pulverization block getter with high gettering efficiency and long service life.

The purpose of the invention is realized as follows: a rolling method of fiber plasticizing gas absorption powder is characterized in that the rolling method of fiber plasticizing gas absorption powder is carried out according to the following steps:

1) preparing raw materials in the air suction alloy according to a certain proportion, preparing the air suction alloy into an alloy by a smelting method, and then crushing and ball-milling the alloy in a protective atmosphere to obtain 325-80 mesh air suction alloy powder;

2) mixing the getter alloy powder with 0.01-2% (mass fraction) of stearic acid uniformly to form alloy powder;

3) uniformly mixing the alloy powder with 0.1-70 wt% of titanium and titanium alloy fibers to form an alloy mixture;

4) performing powder rolling on the alloy mixture at room temperature through a rolling mill to form a rolled plate;

5) and (3) performing vacuum sintering on the rolled plate in a vacuum environment with the vacuum degree of 3-6 x 10 < -3 > Pa to obtain the fiber plasticizing air-breathing rolled plate.

Compared with the prior art, the invention has the advantages that: compared with the traditional rolling method of the getter powder without adding fiber plasticization, the getter material with fiber plasticization has better plasticity, the defect that the technology needs to add some additives such as organic solvent in the powder for some brittle powder and the like to compensate is overcome, and the organic solvent is easy to be carbonized, so that the impurities of the getter material are increased. The method for plasticizing by adding the fibers into the air suction powder enables the forming to be easy in the rolling process; the fiber plasticizing air suction powder rolling forming has the characteristics of short process flow, energy conservation, lower cost, accurate and controllable pressed compact or product components and higher yield. The yield is increased, the cost is reduced, and the method is favorable for large-scale production. The produced air suction plate has better toughness and is not easy to generate the phenomenon of powder falling in use. Can maintain better vacuum degree under the vibration environment, is favorable to components and parts increase of service life. The product produced by the method can meet the shape requirements of large size and over specification of the vacuum air suction material used for the vacuum heat insulation plate in industrial transportation and marine transportation. The mass production is realized.

As a preferable mode of the present invention, the kinds of the alloy include:

a) Zr-Al alloy, Zr-Al-RE alloy, Zr-Al-TE-RE alloy, wherein TE comprises transition group elements of Ti, Fe, Co, Ni, Mn, Pd, Ru, Pt, V, Cr, Nb, Mo, Tc, Rh, Hf, Ta, W, Re, Os and Ir;

b) Zr-C alloy, Zr-C-RE alloy, Zr-C-TE-RE alloy, wherein TE comprises transition group elements of Ti, Fe, Co, Ni, Mn, Pd, Ru, Pt, V, Cr, Nb, Mo, Tc, Rh, Hf, Ta, W, Re, Os and Ir;

c) Zr-V-Fe alloy, Zr-V-Fe-RE alloy, Zr-V-Fe-TE alloy, Zr-V-Fe-RE-TE alloy, wherein TE comprises transition elements of Ti, Co, Ni, Mn, Pd, Ru, Pt, Cr, Nb, Mo, Tc, Rh, Hf, Ta, W, Re, Os and Ir;

d) Zr-Co alloy, Zr-Co-RE alloy, Zr-Co-TE alloy, Zr-Co-RE-TE alloy, wherein TE comprises transition group elements of Ti, Fe, Ni, Mn, Pd, Ru, Pt, V, Cr, Nb, Mo, Tc, Rh, Hf, Ta, W, Re, Os and Ir;

e) Ti-Mo alloy, Ti-Mo-RE alloy, Ti-Mo-TE alloy, Ti-Mo-RE-TE alloy, wherein TE comprises transition group elements of Zr, Fe, Co, Ni, Mn, Pd, Ru, Pt, V, Cr, Nb, Tc, Rh, Hf, Ta, W, Re, Os and Ir;

f) Ti-Zr-V alloy, Ti-Zr-V-RE alloy, Ti-Zr-V-TE-RE alloy, wherein TE comprises transition group elements of Fe, Co, Ni, Mn, Pd, Ru, Pt, Cr, Nb, Mo, Tc, Rh, Hf, Ta, W, Re, Os and Ir;

g) Zr-Co-Re (rhenium) alloy, Zr-Co-Re-RE-TE alloy, wherein TE comprises transition elements of Ti, Fe, Co, Ni, Mn, Pd, Ru, Pt, V, Cr, Nb, Mo, Tc, Rh, Hf, Ta, W, Os and Ir.

As a further preferable mode of the present invention, the RE includes rare earth elements Y, Sc, La, Ce, Pr, Nd, Pm, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb, Lu.

In a further preferred embodiment of the present invention, the titanium or titanium alloy fibers have a diameter of 0.04 to 0.09 mm and a length of 0.01 to 2 mm.

In a further preferred embodiment of the present invention, the ratio of the titanium and titanium alloy fibers is 0.1 to 70 wt%.

In a further preferable scheme of the invention, the rolling pressure of the rolling mill is 10-120 kN, the rolling speed is 1-5 m/min, and the roll gap is 1-4 mm.

As a further preferable scheme of the invention, the sintering process of the rolled plate is to keep the temperature at 1000-1200 ℃ for 0.2-2 h.

Drawings

Figure 1 is a schematic drawing of the rolling and sintering of a fibrous plasticised getter material.

Wherein, 1 alloy powder, 2 rolling mills and 3 fiber plasticizing suction rolling plates.

Detailed Description

The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.

A rolling method of fiber plasticizing gas absorption powder is characterized in that the rolling method of fiber plasticizing gas absorption powder is carried out according to the following steps:

1) preparing raw materials in the air suction alloy according to a certain proportion, preparing the air suction alloy into an alloy by a smelting method, and then crushing and ball-milling the alloy in a protective atmosphere to obtain 325-80 mesh air suction alloy powder;

2) mixing the getter alloy powder with 0.01-2% (mass fraction) of stearic acid uniformly to form alloy powder;

3) uniformly mixing the alloy powder with 0.1-70 wt% of titanium and titanium alloy fibers to form an alloy mixture;

4) performing powder rolling on the alloy mixture at room temperature through a rolling mill to form a rolled plate;

5) and (3) performing vacuum sintering on the rolled plate in a vacuum environment with the vacuum degree of 3-6 x 10 < -3 > Pa to obtain the fiber plasticizing air-breathing rolled plate.

The kinds of the above alloys include:

a) Zr-Al alloy, Zr-Al-RE alloy, Zr-Al-TE-RE alloy, wherein TE comprises transition group elements of Ti, Fe, Co, Ni, Mn, Pd, Ru, Pt, V, Cr, Nb, Mo, Tc, Rh, Hf, Ta, W, Re, Os and Ir;

b) Zr-C alloy, Zr-C-RE alloy, Zr-C-TE-RE alloy, wherein TE comprises transition group elements of Ti, Fe, Co, Ni, Mn, Pd, Ru, Pt, V, Cr, Nb, Mo, Tc, Rh, Hf, Ta, W, Re, Os and Ir;

c) Zr-V-Fe alloy, Zr-V-Fe-RE alloy, Zr-V-Fe-TE alloy, Zr-V-Fe-RE-TE alloy, wherein TE comprises transition elements of Ti, Co, Ni, Mn, Pd, Ru, Pt, Cr, Nb, Mo, Tc, Rh, Hf, Ta, W, Re, Os and Ir;

d) Zr-Co alloy, Zr-Co-RE alloy, Zr-Co-TE alloy, Zr-Co-RE-TE alloy, wherein TE comprises transition group elements of Ti, Fe, Ni, Mn, Pd, Ru, Pt, V, Cr, Nb, Mo, Tc, Rh, Hf, Ta, W, Re, Os and Ir;

e) Ti-Mo alloy, Ti-Mo-RE alloy, Ti-Mo-TE alloy, Ti-Mo-RE-TE alloy, wherein TE comprises transition group elements of Zr, Fe, Co, Ni, Mn, Pd, Ru, Pt, V, Cr, Nb, Tc, Rh, Hf, Ta, W, Re, Os and Ir;

f) Ti-Zr-V alloy, Ti-Zr-V-RE alloy, Ti-Zr-V-TE-RE alloy, wherein TE comprises transition group elements of Fe, Co, Ni, Mn, Pd, Ru, Pt, Cr, Nb, Mo, Tc, Rh, Hf, Ta, W, Re, Os and Ir;

g) Zr-Co-Re (rhenium) alloy, Zr-Co-Re-RE-TE alloy, wherein TE comprises transition elements of Ti, Fe, Co, Ni, Mn, Pd, Ru, Pt, V, Cr, Nb, Mo, Tc, Rh, Hf, Ta, W, Os and Ir.

The RE comprises rare earth elements of Y, Sc, La, Ce, Pr, Nd, Pm, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb and Lu.

The titanium and titanium alloy fibers have a diameter of 0.04 to 0.09 mm and a length of 0.01 to 2 mm.

The weight ratio of the titanium and the titanium alloy fiber is 0.1-70 wt%.

The rolling pressure of the rolling mill is 10-120 kN, the rolling speed is 1-5 m/min, and the roll gap is 1-4 mm.

The sintering process of the rolled plate is to keep the temperature at 1000-1200 ℃ for 0.2-2 h.