阅读说明：本技术 一种提高精密仪器仪表用高纯铍材尺寸稳定性的方法 (Method for improving dimensional stability of high-purity beryllium material for precision instruments and meters ) 是由 肖来荣 任鹏禾 赵小军 蔡圳阳 涂晓萱 张亚芳 于 2021-08-15 设计创作，主要内容包括：一种提高精密仪器仪表用高纯铍材尺寸稳定性的方法,对等静压高纯铍材进行多级时效处理,包括：将等静压高纯铍材加热至100～200℃,保温60～180min,然后使等静压高纯铍材随炉冷却至室温；加热至300～400℃,保温10～30min；再加热至700～900℃,保温30～300min；然后随炉冷却至300～400℃,保温10～30min,最后使等静压高纯铍材随炉冷却至室温；多级时效处理过程中对等静压高纯铍材施加波长0.05～0.20nm,管电压20～50kV,管电流1～10mA的X射线辐照。本发明可得到空位与位错缺陷少、杂质元素与杂质相稳定、残余应力小、尺寸稳定性极高的高纯铍材。(A method for improving the dimensional stability of high-purity beryllium used for precise instruments and meters comprises the following steps of: heating the isostatic high-purity beryllium material to 100-200 ℃, preserving the heat for 60-180 min, and then cooling the isostatic high-purity beryllium material to room temperature along with the furnace; heating to 300-400 ℃, and preserving heat for 10-30 min; then heating to 700-900 ℃, and preserving heat for 30-300 min; then cooling to 300-400 ℃ along with the furnace, preserving heat for 10-30 min, and finally cooling the isostatic high-purity beryllium material to room temperature along with the furnace; and in the process of multistage aging treatment, X-ray irradiation with the wavelength of 0.05-0.20 nm, the tube voltage of 20-50 kV and the tube current of 1-10 mA is applied to isostatic pressing high-purity beryllium materials. The invention can obtain high-purity beryllium material with few vacancy and dislocation defects, stable impurity elements and impurity phases, small residual stress and extremely high dimensional stability.)

1. The method for improving the dimensional stability of the high-purity beryllium material for the precision instruments and meters is characterized in that multistage aging treatment is carried out on the isostatic high-purity beryllium material, and the multistage aging treatment comprises the following steps:

a first time effect processing stage: heating the isostatic pressing high-purity beryllium material to 100-200 ℃, preserving the heat for 60-180 min, and then cooling the isostatic pressing high-purity beryllium material to room temperature along with a furnace;

and a second aging treatment stage: heating the isostatic pressing high-purity beryllium material obtained in the first time-effect treatment stage to 300-400 ℃, and preserving heat for 10-30 min;

and a third aging treatment stage: heating the isostatic high-purity beryllium material obtained in the second aging treatment stage to 700-900 ℃, and preserving heat for 30-300 min;

and a fourth time effect processing stage: cooling the isostatic high-purity beryllium material obtained in the third aging treatment stage to 300-400 ℃ along with the furnace, preserving the heat for 10-30 min, and finally cooling the isostatic high-purity beryllium material to room temperature along with the furnace;

and in the multistage aging treatment process, X-ray irradiation with the wavelength of 0.05-0.20 nm, the tube voltage of 20-50 kV and the tube current of 1-10 mA is applied to the isostatic high-purity beryllium material.

2. The method for improving the dimensional stability of the high-purity beryllium material for the precision instruments and meters as claimed in claim 1, wherein the thickness of the isostatic high-purity beryllium material is less than 2 mm.

3. The method for improving the dimensional stability of the high-purity beryllium material for the precision instruments and meters as claimed in claim 1, wherein the dimensional change of the isostatic high-purity beryllium material after the multistage aging treatment and the X-ray irradiation is not more than 0.0005% after being placed at room temperature for one year.

4. The method for improving the dimensional stability of the high-purity beryllium material for the precision instruments and meters as claimed in claim 1, wherein the dynamic dimensional change rate of the isostatic high-purity beryllium material subjected to the multistage aging treatment and the X-ray irradiation is less than 0.001% under the force-free load.

5. The method for improving the dimensional stability of the high-purity beryllium material for the precise instruments and meters as claimed in claim 1, wherein in the first time-effect treatment stage, the isostatic pressing high-purity beryllium material preliminarily releases residual stress to obtain a metastable state; and cooling the steel plate to room temperature along with the furnace to obtain the permanent deformation.

6. The method for improving the dimensional stability of the high-purity beryllium material for the precision instruments and meters as claimed in claim 1, wherein the X-ray irradiation makes the isostatic high-purity beryllium material in the multistage aging process change the mutual diffusion rate of the components and accelerate the diffusion of impurity elements Fe, Co, Al, Cu and Mn in the isostatic high-purity beryllium material from the matrix into the grain boundary.

Technical Field

The invention relates to a method for improving the dimensional stability of a high-purity beryllium material for a precision instrument, belonging to the technical field of powder metallurgy material processing.

Background

The high-purity beryllium material is strategic and critical, has the largest specific stiffness, the largest specific heat capacity, the best heat-conducting property and the largest thermal neutron cross-section scattering in all metals, and is widely applied to the field of precise instruments and meters. The application environment of a precise instrument has extremely high requirements on the dimensional stability of the high-purity beryllium material, and particularly, the change of an organization structure and a stress state can occur in high-temperature, low-temperature and alternating-temperature environments, so that the reliability and the stability of the high-purity beryllium material are influenced, the precision and the sensitivity of the whole device are obviously reduced, and the service life of the device is obviously prolonged. Therefore, the thermal expansion coefficient and dimensional stability of beryllium are critical to the precision, lifetime, and reliability of precision instruments.

Currently, heat treatment is the traditional method for improving the dimensional stability of beryllium materials. The high-purity beryllium material is heated to a certain temperature and is subjected to heat preservation for aging treatment or cold-hot circulation treatment within a certain temperature range, so that the residual stress is reduced, and the dimensional stability is improved. The single heat treatment method mainly has two defects: because the elastic modulus of the hard phase BeO particles of the high-purity beryllium material is greatly different from that of the substrate, stress concentration is easily caused at an interface, so that cracking is generated, the compactness and stable and reliable performance of the high-purity beryllium material are influenced, and the stability of the structure and the stress of the high-purity beryllium material cannot be considered simultaneously by adopting a single treatment mode; the improvement of the dimensional stability of the high-purity beryllium material is a result of the combined action of the microstructure stability and the residual stress elimination of the high-purity beryllium material, and although a relatively stable microstructure can be obtained by a heat treatment method, the improvement of the dimensional stability of the high-purity beryllium material has certain limitation on effectively eliminating the residual stress in the high-purity beryllium material.

In view of the above, a new technical solution is needed to improve the dimensional stability of high-purity beryllium for precision instruments and meters.

Disclosure of Invention

The invention aims to provide a method for improving the dimensional stability of a high-purity beryllium material for a precision instrument, which can obtain the high-purity beryllium material with few defects such as vacancies, dislocation and the like, stable impurity elements and impurity phases, small residual stress and extremely high dimensional stability.

The technical scheme for solving the technical problems is as follows: a method for improving the dimensional stability of high-purity beryllium material for precision instruments and meters comprises the following steps of performing multistage aging treatment on isostatic high-purity beryllium material, wherein the multistage aging treatment comprises the following steps:

a first time effect processing stage: heating the isostatic pressing high-purity beryllium material to 100-200 ℃, preserving the heat for 60-180 min, and then cooling the isostatic pressing high-purity beryllium material to room temperature along with a furnace;

and a second aging treatment stage: heating the isostatic high-purity beryllium material obtained in the first time-effect treatment stage to 300-400 ℃, and preserving heat for 10-30 min;

and a third aging treatment stage: heating the isostatic high-purity beryllium material obtained in the second aging treatment stage to 700-900 ℃, and preserving heat for 30-300 min;

and a fourth time effect processing stage: cooling the isostatic high-purity beryllium material obtained in the third aging treatment stage to 300-400 ℃ along with the furnace, preserving the heat for 10-30 min, and finally cooling the isostatic high-purity beryllium material to room temperature along with the furnace;

and in the multistage aging treatment process, X-ray irradiation with the wavelength of 0.05-0.20 nm, the tube voltage of 20-50 kV and the tube current of 1-10 mA is applied to the isostatic high-purity beryllium material.

Specifically, the aging treatment process is a solid phase transition process, which is a process of precipitation, desolvation, nucleation and growth of second phase particles from a supersaturated solid solution. Actually, in the process of desolvation of the supersaturated solid solution, a balanced desolvation phase is not directly separated out, but a solute atom segregation region is formed firstly, then a transition phase is separated out, and finally a balanced desolvation precipitation phase is formed; the driving force for the entire process is also the free energy difference.

The influence of partial residual stress on the dimensional stability of the high-purity beryllium material can be only eliminated by adopting conventional stress relief annealing treatment and cold-hot circulation treatment; the precipitated phase of the high-purity beryllium material can be effectively stabilized by adopting high-temperature solution treatment and high-temperature aging, but the crystal grains can be coarsened, and the residual stress is superposed in the cooling process, so that the purposes of effectively removing the residual stress and improving the structure stability cannot be simultaneously achieved by adopting the methods of stress-relief annealing, cold-hot circulation, high-temperature solution, high-temperature aging and the like alone, and the great dimensional instability can be still caused in the subsequent application process.

As a preferable scheme of the method for improving the dimensional stability of the high-purity beryllium material for the precision instruments and meters, the thickness of the isostatic high-purity beryllium material is less than 2 mm.

As a preferred scheme of the method for improving the dimensional stability of the high-purity beryllium material for the precision instruments and meters, the isostatic high-purity beryllium material subjected to the multistage aging treatment and the X-ray irradiation is placed at room temperature for one year, and the dimensional change is not more than 0.0005%.

As a preferred scheme of the method for improving the dimensional stability of the high-purity beryllium material for the precision instruments and meters, the dynamic dimensional change rate of the isostatic high-purity beryllium material subjected to the multistage aging treatment and the X-ray irradiation is less than 0.001% under the condition of no force load.

As a preferred scheme of the method for improving the dimensional stability of the high-purity beryllium material for the precision instruments and meters, in the first time-efficiency treatment stage, the isostatic pressing high-purity beryllium material preliminarily releases residual stress to obtain a metastable state; and cooling the steel plate to room temperature along with the furnace to obtain the permanent deformation.

As a preferable scheme of the method for improving the dimensional stability of the high-purity beryllium material for the precision instruments and meters, the X-ray irradiation enables the isostatic high-purity beryllium material in the multistage aging treatment process to change the mutual diffusion rate of components and accelerate the diffusion of impurity elements such as Fe, Co, Al, Cu, Mn and the like in the isostatic high-purity beryllium material from a base body into a grain boundary.

According to the invention, the high-purity beryllium material is treated by adopting the X-ray irradiation and the multistage aging method, so that the impurity elements Fe and Al in the high-purity beryllium material can be effectively promoted to form a stable precipitated phase on a crystal boundary, the structure stability of the high-purity beryllium material is improved, the residual stress in the high-purity beryllium material can be further reduced, and the dimensional stability of the high-purity beryllium material is improved.

The invention carries out low-temperature aging treatment before the multi-stage aging treatment, namely the first aging treatment stage. The purpose is two-sided: on the first hand, pretreatment is carried out, so that the residual stress in the high-purity beryllium material is primarily released, and a metastable state is obtained; and (5) obtaining the permanent deformation after cooling, and estimating the dimensional stability of the isostatic pressing high-purity beryllium material. And then, on the basis that the multi-stage aging is substantially single-stage aging, adding a temperature rising step (heating to 300-400 ℃ and preserving heat for 10-30 min) and a temperature reducing step (cooling to 300-400 ℃ along with the furnace and preserving heat for 10-30 min) to ensure that the thermal stress in the process is completely eliminated. The subsequent aging temperature and time (700-900 ℃, and the heat preservation time is 30-300 min) are the key.

Under the action of heat at 700-900 ℃, on one hand, microscopic regions such as inter-grain or intra-grain inter-sub-crystal regions are subjected to plastic deformation (when the stress exceeds the yield strength of the material at the temperature) or a relaxation process (when the stress is less than the yield strength of the material at the temperature) so as to release residual stress; on the other hand, atoms acquire energy and have higher vibration frequency, so that lattice distortion energy can be efficiently released, the atoms are gradually converted into an equilibrium state from an original stretched or compressed state, and the effects of residual stress release and lattice relaxation are achieved.

In the invention, the X-ray irradiation plays a role in providing extra energy or reducing a threshold value, but the effect can be fully played within a certain temperature range, the X-ray irradiation cannot play a role below 700 ℃, beryllium materials are easy to have coarse grains and expand structural stress above 900 ℃, and the heat preservation time is difficult to control. And in the third aging treatment stage, the isostatic-pressing high-purity beryllium material obtained in the second aging treatment stage is heated to 700-900 ℃.

The X-rays act on the substance essentially as a transfer of energy, similar to conventional physical fields (temperature field, force field). However, compared with the traditional energy, the action mechanism of the material is different, the X-ray changes the phase change by influencing the motion state of electrons in the substance, and the macroscopic property and the microstructure of the material are closely related to the motion state of the electrons.

In the invention, the influence of X-ray on solid phase aging is mainly as follows:

firstly, the diffusion rate of the components is changed in the aging process due to the difference of free energy generated by substance diffusion or the influence of X-rays on the diffusion frequency of the components, after aging treatment under the X-rays, the components Be are non-ferromagnetic and have no obvious reduction on the free energy, so that more Fe, Co, Al, Cu and Mn elements are accelerated to diffuse into a crystal boundary from a matrix, the dissolution activation energy is reduced, the dissolution is promoted, the precipitation and dissolution temperatures of all precipitation phases move to low-temperature positions, and the aging process is accelerated;

secondly, in the aging precipitation process of the supersaturated solid solution, due to the energy infiltration of the rectangular wave magnetic field in a short time, electromagnetic energy acts in the supersaturated solid solution in the form of magnetic potential energy and impacts the nucleation energy barrier with energy, the free energy required by jumping over the nucleation energy barrier is reduced, the solid state nucleation rate is increased, the aging process is shortened to be within 1h from the traditional 12h or even longer time, and the aging precipitation process is accelerated;

third, the X-rays can accelerate the thermal vibration of the alloy atoms, reduce the potential barrier for the atoms to jump out of the normal lattice position, promote vacancy formation, and increase the average size of vacancies in the alloy. When X-rays are applied to the alloy under the conditions of different aging temperatures, the thermal vibration of atoms is intensified, the formation energy and the migration activation energy of vacancies are reduced, and the movement of the vacancies is promoted while the concentration of the vacancies is increased. When the new phase crystal nucleus is precipitated in an aging mode, the elastic distortion can be caused to increase the nucleation potential energy, and the elastic distortion can be counteracted in a distortion area by the vacancy and other point defects, so that the nucleation potential energy is reduced, and the nucleation rate is increased.

In the present invention, the influence of X-rays on the release of residual stress is mainly:

firstly, on one hand, more Fe, Co, Al, Cu and Mn elements are accelerated to diffuse from a matrix and enter a crystal boundary to promote the nucleation and precipitation of impurity elements and impurity phases on the crystal boundary, and on the other hand, the X rays increase the vacancy concentration to counteract the elastic distortion, and the vacancy concentration and the elastic distortion act simultaneously to promote the lattice relaxation and efficiently release the lattice distortion energy, so that the microscopic residual stress is rapidly reduced;

secondly, the thermal vibration of atoms is further accelerated by X-rays, the atoms are rapidly converted from an original tensile or compressive state to an equilibrium state, and the effects of residual stress release and lattice relaxation are more efficiently achieved.

According to the invention, through X-ray irradiation in cooperation with multistage aging treatment, the tissue stability of the high-purity beryllium material can be obviously improved, and the residual stress in the material is reduced; compared with a single heat treatment mode, the X-ray irradiation synergistic multistage aging treatment has the advantages of more stable component size, shorter experimental period, higher efficiency, low energy consumption and no pollution. The method has the advantages of simple and convenient operation process, low cost, simple process flow, stable structure and small residual stress of the treated high-purity beryllium material, and has very positive effects of improving the precision and the service life of the precision instruments and meters in China.

Drawings

In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below. It should be apparent that the drawings in the following description are merely exemplary, and that other embodiments can be derived from the drawings provided by those of ordinary skill in the art without inventive effort.

The structures, ratios, sizes, and the like shown in the present specification are only used for matching with the contents disclosed in the specification, so that those skilled in the art can understand and read the present invention, and do not limit the conditions for implementing the present invention, so that the present invention has no technical significance, and any structural modifications, changes in the ratio relationship, or adjustments of the sizes, without affecting the functions and purposes of the present invention, should still fall within the scope of the present invention.

FIG. 1 is an environmental scanning electron microscope image of high-purity beryllium material for precision instruments and meters obtained by applying the method;

FIG. 2 is an electron back scattering diffraction diagram of a high-purity beryllium material for precision instruments and meters obtained by applying the method;

FIG. 3 is a metallographic microscope photograph of a high-purity beryllium material for a precision instrument obtained by applying the method of the present invention.

Detailed Description

In order to make the aforementioned objects, features and advantages of the present invention comprehensible, embodiments accompanied with figures are described in detail below. In the following description, numerous specific details are set forth in order to provide a thorough understanding of the present invention. This invention may, however, be embodied in many different forms and should not be construed as limited to the embodiments set forth herein.

Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. The terminology used herein in the description of the invention is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention.

Example 1

The embodiment 1 of the invention provides a method for improving the dimensional stability of a high-purity beryllium material for a precision instrument, which is used for carrying out multistage aging treatment on a isostatic high-purity beryllium material, wherein the multistage aging treatment comprises the following steps:

a first time effect processing stage: heating the isostatic pressing high-purity beryllium material to 150 ℃, preserving the temperature for 180min, and then cooling the isostatic pressing high-purity beryllium material to room temperature along with the furnace;

and a second aging treatment stage: heating the isostatic pressing high-purity beryllium material obtained in the first time-effect treatment stage to 350 ℃, and preserving heat for 20 min;

and a third aging treatment stage: heating the isostatic high-purity beryllium material obtained in the second aging treatment stage to 800 ℃, and preserving the temperature for 180 min;

and a fourth time effect processing stage: cooling the isostatic high-purity beryllium material obtained in the third aging treatment stage to 350 ℃ along with the furnace, preserving the heat for 20min, and finally cooling the isostatic high-purity beryllium material to room temperature along with the furnace;

and in the multistage aging treatment process, X-ray irradiation with the wavelength of 0.10nm, the tube voltage of 30kV and the tube current of 5mA is applied to the isostatic high-purity beryllium material.

The dimensional change of the high-purity beryllium material obtained in example 1 after being left at room temperature for one year was 0.0002%. The dynamic dimensional change under no force load (permanent rate of change in dimension after 50 temperature cycles at room temperature to 200 ℃) was 0.0005%.

Example 2

The embodiment 2 of the invention provides a method for improving the dimensional stability of a high-purity beryllium material for a precision instrument, which is used for carrying out multistage aging treatment on a isostatic high-purity beryllium material, wherein the multistage aging treatment comprises the following steps:

a first time effect processing stage: heating the isostatic pressing high-purity beryllium material to 180 ℃, preserving the heat for 150min, and then cooling the isostatic pressing high-purity beryllium material to room temperature along with the furnace;

and a second aging treatment stage: heating the isostatic pressing high-purity beryllium material obtained in the first time-effect treatment stage to 380 ℃, and preserving heat for 10 min;

and a third aging treatment stage: heating the isostatic high-purity beryllium material obtained in the second aging treatment stage to 850 ℃, and preserving heat for 240 min;

and a fourth time effect processing stage: cooling the isostatic high-purity beryllium material obtained in the third aging treatment stage to 380 ℃ along with the furnace, preserving the heat for 10min, and finally cooling the isostatic high-purity beryllium material to room temperature along with the furnace;

and in the multistage aging treatment process, X-ray irradiation with the wavelength of 0.15nm, the tube voltage of 40kV and the tube current of 8mA is applied to the isostatic high-purity beryllium material.

The dimensional change of the high-purity beryllium material obtained in example 2 after standing at room temperature for one year was 0.0003%. The dynamic dimensional change under no force load (permanent rate of change in dimension after 50 temperature cycles at room temperature to 200 ℃) was 0.0008%.

Example 3

The embodiment 3 of the invention provides a method for improving the dimensional stability of a high-purity beryllium material for a precision instrument, which is used for carrying out multistage aging treatment on a isostatic high-purity beryllium material, wherein the multistage aging treatment comprises the following steps:

a first time effect processing stage: heating the isostatic pressing high-purity beryllium material to 120 ℃, preserving the temperature for 90min, and then cooling the isostatic pressing high-purity beryllium material to room temperature along with the furnace;

and a second aging treatment stage: heating the isostatic pressing high-purity beryllium material obtained in the first time-effect treatment stage to 320 ℃, and preserving heat for 20 min;

and a third aging treatment stage: heating the isostatic high-purity beryllium material obtained in the second aging treatment stage to 750 ℃, and preserving heat for 240 min;

and a fourth time effect processing stage: cooling the isostatic high-purity beryllium material obtained in the third aging treatment stage to 320 ℃ along with the furnace, preserving the heat for 20min, and finally cooling the isostatic high-purity beryllium material to room temperature along with the furnace;

and in the multistage aging treatment process, X-ray irradiation with the wavelength of 0.05nm, the tube voltage of 20kV and the tube current of 6mA is applied to the isostatic high-purity beryllium material.

The dimensional change of the high-purity beryllium material obtained in example 3 after standing at room temperature for one year was 0.0004%. The dynamic dimensional change under no force load (permanent rate of change in dimension after 50 temperature cycles at room temperature to 200 ℃) was 0.0009%.

Comparative example 1

Comparative example 1 was compared with example 3, a comparative test without X-ray co-treatment.

Heating isostatic high-purity beryllium material to 120 ℃, preserving heat for 90min, and then cooling to room temperature along with the furnace. Then, heating the isostatic high-purity beryllium material to 320 ℃, and preserving the heat for 20 min; then heating to 750 ℃, preserving heat for 240min, then cooling to 320 ℃ with the furnace, preserving heat for 20min, and finally cooling to room temperature with the furnace. The dimensional change of the product after standing at room temperature for one year is 0.0081%. The dynamic dimensional change under no force load (permanent rate of change in dimension after 50 temperature cycles from room temperature to 200 ℃) was 0.0044%.

Comparative example 2

Comparative example 2 is compared with example 3, replacing the electromagnetic wave in the form of X-rays with the electromagnetic wave in the form of electric current.

Applying 50A of direct current in the aging process of isostatic pressing high-purity beryllium material; heating isostatic high-purity beryllium material to 120 ℃, preserving heat for 90min, and then cooling to room temperature along with the furnace. Then, heating the isostatic high-purity beryllium material to 320 ℃, and preserving the heat for 20 min; then heating to 750 ℃, preserving heat for 240min, then cooling to 320 ℃ with the furnace, preserving heat for 20min, and finally cooling to room temperature with the furnace. The dimensional change of the product after standing at room temperature for one year is 0.0084%. The dynamic dimensional change under no force load (permanent rate of change in dimension after 50 temperature cycles at room temperature to 200 ℃) was 0.0051%.

Example 4

The embodiment 4 of the invention provides a method for improving the dimensional stability of a high-purity beryllium material for a precision instrument, which is used for carrying out multistage aging treatment on a isostatic high-purity beryllium material, wherein the multistage aging treatment comprises the following steps:

a first time effect processing stage: heating the isostatic pressing high-purity beryllium material to 150 ℃, preserving the heat for 150min, and then cooling the isostatic pressing high-purity beryllium material to room temperature along with the furnace;

and a second aging treatment stage: heating the isostatic pressing high-purity beryllium material obtained in the first time-effect treatment stage to 360 ℃, and preserving heat for 30 min;

and a third aging treatment stage: heating the isostatic high-purity beryllium material obtained in the second aging treatment stage to 800 ℃, and preserving heat for 200 min;

and a fourth time effect processing stage: cooling the isostatic high-purity beryllium material obtained in the third aging treatment stage to 350 ℃ along with the furnace, preserving the heat for 10min, and finally cooling the isostatic high-purity beryllium material to room temperature along with the furnace;

and in the multistage aging treatment process, X-ray irradiation with the wavelength of 0.15nm, the tube voltage of 30kV and the tube current of 8mA is applied to the isostatic high-purity beryllium material.

The dimensional change of the high-purity beryllium material obtained in example 4 after one year of standing at room temperature was 0.0003%. The dynamic dimensional change under no force load (permanent rate of change in dimension after 50 temperature cycles at room temperature to 200 ℃) was 0.0006%.

Comparative example 3

Comparative example 3 was compared with example 4, comparative test without X-ray co-treatment.

Heating isostatic high-purity beryllium material to 150 ℃, preserving heat for 150min, and then cooling to room temperature along with the furnace. Then heating the isostatic high-purity beryllium material to 360 ℃, and preserving the heat for 30 min; then heating to 800 ℃, preserving heat for 200min, then cooling to 350 ℃ with the furnace, preserving heat for 10min, and finally cooling to room temperature with the furnace. The dimensional change of the product after standing at room temperature for one year is 0.0093%. The dynamic dimensional change under no force load (permanent rate of change in dimension after 50 temperature cycles at room temperature to 200 ℃) was 0.0062%.

Comparative example 4

Comparative example 4 and example 4 were compared, and electromagnetic waves in the form of magnetic field were substituted for electromagnetic waves in the form of X-ray.

Applying a static magnetic field of 0.1T in the aging process of the isostatic pressing high-purity beryllium material; heating isostatic high-purity beryllium material to 150 ℃, preserving heat for 150min, and then cooling to room temperature along with the furnace. Then heating the isostatic high-purity beryllium material to 360 ℃, and preserving the heat for 30 min; then heating to 800 ℃, preserving heat for 200min, then cooling to 350 ℃ with the furnace, preserving heat for 10min, and finally cooling to room temperature with the furnace. The dimensional change of the product after standing at room temperature for one year is 0.0088%. The dynamic dimensional change under no force load (permanent rate of change in dimension after 50 temperature cycles from room temperature to 200 ℃) was 0.0041%.

Example 5

The embodiment 5 of the invention provides a method for improving the dimensional stability of a high-purity beryllium material for a precision instrument, which is used for carrying out multistage aging treatment on a isostatic high-purity beryllium material, wherein the multistage aging treatment comprises the following steps:

a first time effect processing stage: heating the isostatic pressing high-purity beryllium material to 180 ℃, preserving the temperature for 120min, and then cooling the isostatic pressing high-purity beryllium material to room temperature along with the furnace;

and a second aging treatment stage: heating the isostatic pressing high-purity beryllium material obtained in the first time-effect treatment stage to 400 ℃, and preserving heat for 10 min;

and a third aging treatment stage: heating the isostatic high-purity beryllium material obtained in the second aging treatment stage to 850 ℃, and preserving heat for 240 min;

and a fourth time effect processing stage: cooling the isostatic high-purity beryllium material obtained in the third aging treatment stage to 300 ℃ along with the furnace, preserving the heat for 10min, and finally cooling the isostatic high-purity beryllium material to room temperature along with the furnace;

and in the multistage aging treatment process, X-ray irradiation with the wavelength of 0.10nm, the tube voltage of 50kV and the tube current of 7mA is applied to the isostatic high-purity beryllium material.

The dimensional change of the high-purity beryllium material obtained in example 5 after one year of standing at room temperature was 0.0004%. The dynamic dimensional change under no force load (permanent rate of change in dimension after 50 temperature cycles at room temperature to 200 ℃) was 0.0005%.

Comparative example 5

Comparative example 5 was compared with example 5, a comparative test without X-ray co-treatment.

Heating isostatic high-purity beryllium material to 180 ℃, preserving heat for 120min, and then cooling to room temperature along with the furnace. Then heating the isostatic high-purity beryllium material to 400 ℃, and preserving the heat for 10 min; then heating to 850 ℃, preserving heat for 240min, then cooling to 300 ℃ with the furnace, preserving heat for 10min, and finally cooling to room temperature with the furnace. The dimensional change was 0.0061% after standing at room temperature for one year. The dynamic dimensional change under no force load (permanent rate of change in dimension after 50 temperature cycles at room temperature to 200 ℃) was 0.0075%.

Comparative example 6

Comparative example 6 compares with example 5, replacing the electromagnetic wave in the form of X-rays with the electromagnetic wave in the form of a magnetic field.

Heating isostatic high-purity beryllium material to 180 ℃, preserving heat for 120min, and then cooling to room temperature along with the furnace. Then heating the isostatic high-purity beryllium material to 400 ℃, and preserving the heat for 10 min; then heating to 850 ℃, preserving heat for 240min, then cooling to 300 ℃ with the furnace, preserving heat for 10min, and finally cooling to room temperature with the furnace. The dimensional change of the product after standing at room temperature for one year is 0.0088%. The dynamic dimensional change under no force load (permanent rate of change in dimension after 50 temperature cycles at room temperature to 200 ℃) was 0.0090%.

Comparative example 7

Comparative example 7 is compared with example 5, and the multistage aging heating mode is selected, and the temperature rise process in the removing stage can not completely eliminate the thermal stress in the heating process.

Applying X-ray irradiation with the wavelength of 0.10nm, the tube voltage of 50kV and the tube current of 7mA in the aging process of the isostatic pressing high-purity beryllium material; heating isostatic high-purity beryllium material to 180 ℃, preserving heat for 120min, and then taking out the beryllium material from the air at room temperature to cool the beryllium material to the room temperature. Then heating to 850 ℃, preserving heat for 240min, then cooling to 300 ℃ along with the furnace, preserving heat for 10min, and then cooling to room temperature along with the furnace. The dimensional change was 0.0006% at room temperature for one year. The dynamic dimensional change under no force load (permanent rate of change in dimension after 50 temperature cycles at room temperature to 200 ℃) was 0.0011%.

Comparative example 8

Comparative example 8 compares with example 5, screens the multistage aging cooling mode, removes the stage cooling process and replaces the furnace cooling with taking out the room temperature air to cool to room temperature, will make the thermal stress in the cooling process can not be completely eliminated.

Applying X-ray irradiation with the wavelength of 0.10nm, the tube voltage of 50kV and the tube current of 7mA in the aging process of the isostatic pressing high-purity beryllium material; heating isostatic high-purity beryllium material to 180 ℃, preserving heat for 120min, and then taking out the beryllium material from the air at room temperature to cool the beryllium material to the room temperature. Then heating the isostatic high-purity beryllium material to 400 ℃, and preserving the heat for 10 min; then heating to 850 ℃, preserving the heat for 240min, and then taking out the mixture from the room temperature air to cool to the room temperature. The dimensional change was 0.0009% at room temperature for one year. The dynamic dimensional change under no force load (permanent rate of change in dimension after 50 temperature cycles at room temperature to 200 ℃) was 0.0012%.

Comparative example 9

Comparative example 9 compares with example 5, screens the specific temperature and holding time of multistage aging, and simultaneously removes the stage heating and stage cooling processes, so that the thermal stress in the treatment process can not be completely eliminated.

Applying X-ray irradiation with the wavelength of 0.10nm, the tube voltage of 50kV and the tube current of 7mA in the aging process of the isostatic pressing high-purity beryllium material; heating isostatic high-purity beryllium material to 180 ℃, preserving heat for 120min, and then cooling to room temperature along with the furnace. And then heating the isostatic high-purity beryllium material to 850 ℃, preserving the heat for 240min, and then cooling the beryllium material to the room temperature along with the furnace. The dimensional change of the film after standing at room temperature for one year is 0.0012 percent. The dynamic dimensional change under no force load (permanent rate of change in dimension after 50 temperature cycles at room temperature to 200 ℃) was 0.0018%.

Comparative example 10

Comparative example 10 is compared with example 5, the specific temperature and heat preservation time of multistage aging are screened, and the parameters of the stage heating and stage cooling processes are changed, so that the thermal stress in the treatment process cannot be completely eliminated.

Applying X-ray irradiation with the wavelength of 0.10nm, the tube voltage of 50kV and the tube current of 7mA in the aging process of the isostatic pressing high-purity beryllium material; heating isostatic high-purity beryllium material to 180 ℃, preserving heat for 120min, and then cooling to room temperature along with the furnace. Then heating the isostatic high-purity beryllium material to 500 ℃, and preserving the heat for 10 min; then heating to 850 ℃, preserving heat for 240min, then cooling to 200 ℃ with the furnace, preserving heat for 10min, and finally cooling to room temperature with the furnace. The dimensional change of the sheet after standing at room temperature for one year is 0.0013%. The dynamic dimensional change under no force load (permanent rate of change in dimension after 50 temperature cycles at room temperature to 200 ℃) was 0.0020%.

Comparative example 11

Comparing the comparative example 11 with the example 5, and screening the specific temperature and the heat preservation time of the multi-stage aging, wherein the maximum temperature of the multi-stage aging is increased from 850 ℃ to 1000 ℃, the crystal grains are coarsened, and the structure stress is increased.

Applying X-ray irradiation with the wavelength of 0.10nm, the tube voltage of 50kV and the tube current of 7mA in the aging process of the isostatic pressing high-purity beryllium material; heating isostatic high-purity beryllium material to 180 ℃, preserving heat for 120min, and then cooling to room temperature along with the furnace. Then heating the isostatic high-purity beryllium material to 400 ℃, and preserving the heat for 10 min; then heating to 1000 ℃, preserving heat for 240min, then cooling to 300 ℃ with the furnace, preserving heat for 10min, and finally cooling to room temperature with the furnace. The dimensional change was 0.0031% at room temperature for one year. The dynamic dimensional change under no force load (permanent rate of change in dimension after 50 temperature cycles from room temperature to 200 ℃) was 0.0045%.

Comparative example 12

And comparing the comparative example 12 with the example 5, and screening the specific temperature and the heat preservation time of the multistage aging, wherein the heat preservation time of the multistage aging is increased from 240min to 360min, the crystal grains are coarsened, and the structure stress is increased.

Applying X-ray irradiation with the wavelength of 0.10nm, the tube voltage of 50kV and the tube current of 7mA in the aging process of the isostatic pressing high-purity beryllium material; heating isostatic high-purity beryllium material to 180 ℃, preserving heat for 120min, and then cooling to room temperature along with the furnace. Then heating the isostatic high-purity beryllium material to 400 ℃, and preserving the heat for 10 min; then heating to 850 ℃, preserving heat for 360min, then cooling to 300 ℃ along with the furnace, preserving heat for 10min, and finally cooling to room temperature along with the furnace. The dimensional change was 0.0021% after standing at room temperature for one year. The dynamic dimensional change under no load (permanent rate of change in dimension after 50 temperature cycles at room temperature to 200 ℃) was 0.0032%.

Referring to fig. 1, 2 and 3, the invention adopts X-ray irradiation in cooperation with multistage aging treatment, and compared with the conventional stress relief annealing or cold-heat cycle treatment method, the optimization technology of the invention improves the dimensional stability of the obtained high-purity beryllium material by one order of magnitude, the dimensional change of the high-purity beryllium material after being placed at room temperature for one year is less than 0.0005%, and the dynamic dimensional change (the permanent dimensional change rate after 50 temperature cycles at room temperature to 200 ℃) under the condition of no force load is less than 0.001%. The invention can obviously improve the tissue stability of the high-purity beryllium material and reduce the residual stress in the material by the X-ray irradiation in cooperation with the multistage aging treatment. Compared with a single heat treatment mode, the X-ray irradiation synergistic multistage aging treatment has the advantages of more stable component size, shorter experimental period, higher efficiency, low energy consumption and no pollution. The method has the advantages of simple and convenient operation process, low cost, simple process flow, stable structure of the treated high-purity beryllium material and small residual stress. Has very positive effect on improving the precision and the service life of the precision instrument and meter in China.

The technical features of the embodiments described above may be arbitrarily combined, and for the sake of brevity, all possible combinations of the technical features in the embodiments described above are not described, but should be considered as being within the scope of the present specification as long as there is no contradiction between the combinations of the technical features.

The above-mentioned embodiments only express several embodiments of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention. Therefore, the protection scope of the present patent shall be subject to the appended claims.