CN106747343A - A kind of preparation method based on surface rapid thermal treatment high-purity compact magnesium oxide target - Google Patents
A kind of preparation method based on surface rapid thermal treatment high-purity compact magnesium oxide target Download PDFInfo
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Abstract
The present invention provides a kind of preparation method based on surface rapid thermal treatment high-purity compact magnesium oxide target, comprises the following steps：With magnesium oxide powder as raw material, with zirconia ball as medium, planetary ball mill is carried out to raw material, the powder after grinding carries out 200 mesh sieves point；Powder after sieve is carried out into cold isostatic compaction and obtains magnesia pressed compact；Magnesia pressed compact is carried out into vacuum-sintering, after vacuum-sintering terminates, surface accurate is carried out according to required target size and is machined to target material surface roughness≤0.8 μm, obtain magnesium oxide target；Magnesium oxide target is carried out into surface grinding, then cleaned, surface rapid thermal treatment finally is carried out with continuous wave laser heat treating process, scanning beam method or non-coherent broad band frequency Light Source Method under vacuum, is obtained based on surface rapid thermal treatment high-purity compact magnesium oxide target.The present invention prepare magnesium oxide target purity is high, good compactness, top layer are consistent with interior layer tissue, and preparation method is simply, short time limit, environment protecting and power-saving.
Description
Technical field
The invention belongs to magnesium oxide target technical field, and in particular to one kind is based on surface rapid thermal treatment high-purity compact oxygen
Change the preparation method of magnesium target.
Background technology
It is good etc. excellent that there is magnesia high high-temp stability, high dielectric property, low-dielectric loss and various substrate lattices to match
Point, magnesia film generally uses magnetically controlled sputter method, and the purity of target, consistency, crystallite dimension and Size Distribution all can poles
Sedimentation rate, sputter coating particle during the consistency influence sputtering of the quality and performance of earth effect sputtered film, such as target
Density and arc discharge, have an effect on the electrical and optical performance of sputter coating, and the crystal grain of target is more tiny, and sputter rate is got over
Hurry up, grain size distribution gets over concentration, thickness distribution is also more uniform.
At present, the preparation method of magnesium oxide target mainly has pressureless sintering, injection forming, hot pressed sintering, high temperature insostatic pressing (HIP) to burn
Knot and cold isostatic compaction etc., but all there is certain defect in these methods.Pressureless sintering is easy to be deformed, target is surrounded and watched
Structure is uneven, yield rate is low, and a large amount of binding agents are used in injection forming, and target purity is low, and easily causes target deformation
Ftracture, high temperature insostatic pressing (HIP) is relatively costly etc..And magnesium oxide target is in mechanical processing process, hardened layer is always introduced, easily made
Into tool wear, and a large amount of dislocations and stress are being introduced in metal surface, increasing top layer roughness and hardness, directly resulting in target
Material sputtering rate and the uniformity of film of initial stage sputtering are poor.Generally for eliminate target material surface hardened layer influence, it is necessary in target
Formally using burning target is preceding carried out, skim-coat is removed in sputtering to material, not only causes spillage of material to target, and consume the substantial amounts of time with
Energy, improves use cost.
A kind of preparation method of hot pressed sintering high-density magnesium oxide target disclosed in Chinese patent CN103030380A, will
High-purity nano level magnesium oxide powder is placed in hot-pressed sintering furnace, is sintered through vacuum, the pressurization that heats up, pressurize lipid oxidation magnesium target
Size reaches design load.The method prepare magnesium oxide target purity is high, consistency is high, but it is relatively costly, technique is more multiple
It is miscellaneous.And currently for magnesium oxide target cementation zone treatment in terms of research it is also rare.
The content of the invention
The technical problem to be solved in the present invention is to provide a kind of based on surface rapid thermal treatment high-purity compact magnesium oxide target
Preparation method, the magnesium oxide powder of high-purity as raw material adds through cold isostatic compaction, vacuum-sintering, surface accurate machine
Work, magnesium oxide target is obtained, then using continuous wave laser heat treating process, scanning beam method or non-coherent broad band frequency Light Source Method
Surface rapid thermal treatment is carried out to target, is obtained based on surface rapid thermal treatment high-purity compact magnesium oxide target.It is prepared by the present invention
Method cycle is short, low production cost, the magnesium oxide target crystal grain of preparation is small, and consistency is high, and purity is high, and preparation engineering is pollution-free,
Material signal is small, environmental protection, is suitable for batch production.
In order to solve the above technical problems, the technical scheme is that：
A kind of preparation method based on surface rapid thermal treatment high-purity compact magnesium oxide target, comprises the following steps：
(1) with magnesium oxide powder as raw material, planetary ball mill is carried out to raw material, rotational speed of ball-mill is 150-300r/min, ball milling
Time is 8-32h, and ratio of grinding media to material is 1.5-3:1, the powder after grinding carries out 200 mesh sieves point；
(2) powder after sieve in step (1) is carried out into cold isostatic compaction, pressure is 150-350MPa, and the dwell time is 5-
20min, obtains magnesia pressed compact；
(3) magnesia pressed compact in step (2) is carried out into vacuum-sintering, sintering temperature is 1400-1550 DEG C, and soaking time is
2-10h, vacuum is 0.1-1.0Pa, after vacuum-sintering terminates, surface accurate machining is carried out according to required target size
To target material surface roughness≤0.8 μm, magnesium oxide target is obtained；
(4) step (3) magnesium oxide target is carried out into surface grinding, is then cleaned, finally under vacuum with company
Continuous ripple LASER HEAT TREATMENT method, scanning beam method or non-coherent broad band frequency Light Source Method carry out surface rapid thermal treatment, are based on
Surface rapid thermal treatment high-purity compact magnesium oxide target.
Used as the preferred of above-mentioned technical proposal, in the step (1), the purity of magnesium oxide powder is not less than 99.99%, miscellaneous
Prime element total content is below 100ppm, and average grain diameter is 100-300nm.
Used as the preferred of above-mentioned technical proposal, in the step (1), ball-milling medium is zirconia ball, the differential middle ball of ball：It is small
Ball is 1-3:1.
Used as the preferred of above-mentioned technical proposal, in the step (2), the relative density of magnesia pressed compact is 58-62%, phase
2% is less than to density variation.
Used as the preferred of above-mentioned technical proposal, in the step (3), the temperature-rise period of vacuum-sintering is：Room temperature is heated to
500-1000 DEG C, 4-10h is incubated, the speed with the rate of heat addition no more than 5 DEG C/min is warmed up to after 1000 DEG C and starts to vacuumize,
Sintering vacuum in 10min is 0.1-1.0Pa, and then the speed with the rate of heat addition no more than 2 DEG C/min heats up from 1000 DEG C
To 1400-1550 DEG C of sintering temperature, 2-10h is incubated.
Used as the preferred of above-mentioned technical proposal, in the step (3), the average grain size of magnesium oxide target is less than 7 μm,
Dimensional discrepancy is less than 3.0 μm, and surface roughness Ra is less than 0.4 μm.
Used as the preferred of above-mentioned technical proposal, in the step (4), cleaning method is：First piece surface is removed with soap lye
Greasy dirt, then be 1 with volume ratio:1:The mixing of the hydrofluoric acid of the sulfuric acid, 12-14wt% nitric acid and 12-14% of 1 24-26wt%
Solution acidic reagent carries out Chemical cleaning, finally removes grease with acetone.
Used as the preferred of above-mentioned technical proposal, in the step (4), the scan mode of continuous wave laser heat treating process is to take
Multiple scanning mode or spiral scan pattern are access to, laser power is 1-3kW, and laser defocus distance is 20-50mm, and spot diameter is
10-50mm, sweep speed is 1-50mm/s, and heating-up temperature is 350-450 DEG C, in scanning process target angle of inclination be 10 °-
30°。
Used as the preferred of above-mentioned technical proposal, in the step (4), the scan mode of scanning beam method is reciprocal to overlap
Scan mode or spiral scan pattern, beam spot power density are 1-3kW/cm2, sweep speed is 1-50mm/s, heating
Speed is 100-200 DEG C/s, and heating-up temperature is 350-450 DEG C.
Used as the preferred of above-mentioned technical proposal, in the step (4), the scan mode of non-coherent broad band frequency Light Source Method is whole
Body radiation mode, non-coherent broad band frequency light source is halogen light lamp, arc lamp, graphite heater or infrared equipment, and the speed of heating is
50-100 DEG C/s, heating-up temperature is 350-450 DEG C, and soaking time is 1-10min.
Compared with prior art, the invention has the advantages that：
(1) what prepared by the present invention uses ball-milling technology treatment based on surface rapid thermal treatment high-purity compact magnesium oxide target
High-purity mangesium oxide magnesium dust improves as raw material, the particle diameter distribution of the magnesium oxide powder after ball-milling treatment, dispersiveness, improves
Intragranular portion distortional strain energy, the density and uniformity of base material are far above traditional unidirectional compression when making cold isostatic compaction or two-way receive
Molded base substrate, can obtain consistency higher through vacuum-sintering at a relatively low sintering temperature afterwards, and crystallite dimension is more tiny
Even target, without additive and sintering aid in sintering process, eliminates the gas pressure for hindering hole to eliminate in stomata, promotees
Enter target densification, and the surface smoothness of target is good, and size is unrestricted greatly.
(2) present invention prepare based on surface rapid thermal treatment high-purity compact magnesium oxide target by continuous wave laser it is hot at
Logos, scanning beam method or non-coherent broad band frequency Light Source Method carry out surface rapid thermal treatment to target, by rapid thermal treatment
Skin effect, recrystallize the hardened layer of target material surface, eliminate hardened layer in stress and dislocation, obtain and matrix base
This consistent recrystallized structure, the cementation zone for solving magnesium oxide target is difficult to the technical problem for eliminating, and does not interfere with target
The interior tissue and cream plate performance of material.
(3) preparation method of the present invention is simple, and with short production cycle, efficiency high, low production cost can be mass, and prepare
Journey is pollution-free, and spillage of material is small, environmental protection, and the magnesium oxide target purity of preparation is high, and good compactness, size is unrestricted, target
The surface of material is consistent with the tissue of inside, and the performance for maintaining target is homogeneous, is suitable for industrialized production.
Specific embodiment
Describe the present invention in detail below in conjunction with specific embodiment, herein illustrative examples of the invention and explanation
It is for explaining the present invention but not as a limitation of the invention.
Embodiment 1：
(1) with magnesium oxide powder as raw material, planetary ball mill is carried out to raw material, ball-milling medium is zirconia ball, during ball is differential
Ball：Bead is 1:1, rotational speed of ball-mill is 200r/min, and Ball-milling Time is 16h, and ratio of grinding media to material is 2:1, the powder after grinding carries out 200
Mesh sieve point, the purity of wherein magnesium oxide powder is not less than 99.99%, and impurity element total content is below 100ppm, average grain diameter
It is 100nm.
(2) powder after sieve is carried out into cold isostatic compaction, pressure is 200MPa, and the dwell time is 8min, obtains magnesia
Pressed compact, the wherein relative density of magnesia pressed compact are 59.7%, and relative density deviation is less than 2%.
(3) magnesia pressed compact is carried out into vacuum-sintering, room temperature is heated to 500 DEG C, 4h is incubated, with 5 DEG C/min of the rate of heat addition
Speed be warmed up to 1000 DEG C after start to vacuumize, the sintering vacuum in 10min be 0.85Pa, then with the rate of heat addition 2
DEG C/speed of min is warmed up to 1400 DEG C of sintering temperature from 1000 DEG C, 4h is incubated, after vacuum-sintering terminates, according to required target chi
Little progress row carries out surface accurate machining and obtains magnesium oxide target, and the wherein average grain size of magnesium oxide target is less than 7 μm, chi
Very little deviation is less than 3.0 μm, and surface roughness Ra is less than 0.4 μm.
(4) magnesium oxide target is carried out into surface grinding, then first removes piece surface greasy dirt with soap lye, then be with volume ratio
1:1:The mixed solution acid reagent of the sulfuric acid, 12wt% nitric acid and 12% hydrofluoric acid of 1 24wt% carries out Chemical cleaning, most
Grease is removed with acetone afterwards, finally surface rapid thermal treatment is carried out with continuous wave laser heat treating process under vacuum, continuously
The scan mode of ripple LASER HEAT TREATMENT method is overlap joint shuttle-scanning mode, and laser power is 2kW, and laser defocus distance is 50mm,
Spot diameter is 13mm, and sweep speed is 40mm/s, and heating-up temperature is 420 DEG C, and target angle of inclination is 15 ° in scanning process,
The light beam for preventing surface from reflecting burns laser head, obtains based on surface rapid thermal treatment high-purity compact magnesium oxide target.
Embodiment 2：
(1) with magnesium oxide powder as raw material, planetary ball mill is carried out to raw material, ball-milling medium is zirconia ball, during ball is differential
Ball：Bead is 1:1, rotational speed of ball-mill is 200r/min, and Ball-milling Time is 16h, and ratio of grinding media to material is 2:1, the powder after grinding carries out 200
Mesh sieve point, the purity of wherein magnesium oxide powder is not less than 99.99%, and impurity element total content is below 100ppm, average grain diameter
It is 100nm.
(2) powder after sieve is carried out into cold isostatic compaction, pressure is 200MPa, and the dwell time is 8min, obtains magnesia
Pressed compact, the wherein relative density of magnesia pressed compact are 59.8%, and relative density deviation is less than 2%.
(3) magnesia pressed compact is carried out into vacuum-sintering, room temperature is heated to 500 DEG C, 4h is incubated, with 5 DEG C/min of the rate of heat addition
Speed be warmed up to 1000 DEG C after start to vacuumize, the sintering vacuum in 10min be 0.85Pa, then with the rate of heat addition 2
DEG C/speed of min is warmed up to 1450 DEG C of sintering temperature from 1000 DEG C, 4h is incubated, after vacuum-sintering terminates, according to required target chi
Little progress row carries out surface accurate machining and obtains magnesium oxide target, and the wherein average grain size of magnesium oxide target is less than 7 μm, chi
Very little deviation is less than 3.0 μm, and surface roughness Ra is less than 0.4 μm.
(4) magnesium oxide target is carried out into surface grinding, then first removes piece surface greasy dirt with soap lye, then be with volume ratio
1:1:The mixed solution acid reagent of the sulfuric acid, 14wt% nitric acid and 14% hydrofluoric acid of 1 26wt% carries out Chemical cleaning, most
Grease is removed with acetone afterwards, finally surface rapid thermal treatment, scanning beam is carried out with scanning beam method under vacuum
The scan mode of method is spiral scan pattern, and beam spot power density is 2kW/cm2, sweep speed is 40mm/s, heating
Speed is 100 DEG C/s, and heating-up temperature is 420 DEG C, and soaking time is 10s, is obtained based on surface rapid thermal treatment high-purity compact oxygen
Change magnesium target.
Embodiment 3：
(1) with magnesium oxide powder as raw material, planetary ball mill is carried out to raw material, ball-milling medium is zirconia ball, during ball is differential
Ball：Bead is 1:1, rotational speed of ball-mill is 150r/min, and Ball-milling Time is 8h, and ratio of grinding media to material is 1.5:1, the powder after grinding is carried out
200 mesh sieves point, the purity of wherein magnesium oxide powder is not less than 99.99%, and impurity element total content is below 100ppm, average grain
Footpath is 300nm.
(2) powder after sieve is carried out into cold isostatic compaction, pressure is 350MPa, and the dwell time is 20min, obtains magnesia
Pressed compact, the wherein relative density of magnesia pressed compact are 62%, and relative density deviation is less than 2%.
(3) magnesia pressed compact is carried out into vacuum-sintering, room temperature is heated to 1000 DEG C, is incubated 4h, and 5 are no more than with the rate of heat addition
DEG C/speed of min starts to vacuumize after being warmed up to 1000 DEG C, the sintering vacuum in 10min is 1.0Pa, then heating
Speed of the speed no more than 2 DEG C/min is warmed up to 1550 DEG C of sintering temperature from 1000 DEG C, is incubated 10h, after vacuum-sintering terminates, root
Surface accurate machining is carried out according to required target size obtain magnesium oxide target, wherein the average crystal grain chi of magnesium oxide target
Very little to be less than 7 μm, dimensional discrepancy is less than 3.0 μm, and surface roughness Ra is less than 0.4 μm.
(4) magnesium oxide target is carried out into surface grinding, then first removes piece surface greasy dirt with soap lye, then be with volume ratio
1:1:The mixed solution acid reagent of the sulfuric acid, 13wt% nitric acid and 13% hydrofluoric acid of 1 25wt% carries out Chemical cleaning, most
Grease is removed with acetone afterwards, finally surface rapid thermal treatment, non-phase is carried out with non-coherent broad band frequency Light Source Method under vacuum
The scan mode of dry broadband frequency Light Source Method is overall radiation mode, and non-coherent broad band frequency light source is halogen light lamp, and the speed of heating is
50 DEG C/s, heating-up temperature is 420 DEG C, and soaking time is 1min, is obtained based on surface rapid thermal treatment high-purity compact magnesium oxide target
Material.
Embodiment 4：
(1) with magnesium oxide powder as raw material, planetary ball mill is carried out to raw material, ball-milling medium is zirconia ball, during ball is differential
Ball：Bead is 3:1, rotational speed of ball-mill is 200r/min, and Ball-milling Time is 14h, and ratio of grinding media to material is 2:1, the powder after grinding carries out 200
Mesh sieve point, the purity of wherein magnesium oxide powder is not less than 99.99%, and impurity element total content is below 100ppm, average grain diameter
It is 150nm.
(2) powder after sieve is carried out into cold isostatic compaction, pressure is 250MPa, and the dwell time is 10min, obtains magnesia
Pressed compact, the wherein relative density of magnesia pressed compact are 59.5%, and relative density deviation is less than 2%.
(3) magnesia pressed compact is carried out into vacuum-sintering, room temperature is heated to 800 DEG C, is incubated 6h, and 5 are no more than with the rate of heat addition
DEG C/speed of min starts to vacuumize after being warmed up to 1000 DEG C, the sintering vacuum in 10min is 0.5Pa, then heating
Speed of the speed no more than 2 DEG C/min is warmed up to 1500 DEG C of sintering temperature from 1000 DEG C, is incubated 2h, after vacuum-sintering terminates, root
Surface accurate machining is carried out according to required target size obtain magnesium oxide target, wherein the average crystal grain chi of magnesium oxide target
Very little to be less than 7 μm, dimensional discrepancy is less than 3.0 μm, and surface roughness Ra is less than 0.4 μm.
(4) magnesium oxide target is carried out into surface grinding, then first removes piece surface greasy dirt with soap lye, then be with volume ratio
1:1:The mixed solution acid reagent of the sulfuric acid, 12wt% nitric acid and 14% hydrofluoric acid of 1 26wt% carries out Chemical cleaning, most
Grease is removed with acetone afterwards, finally surface rapid thermal treatment is carried out with continuous wave laser heat treating process under vacuum, continuously
The scan mode of ripple LASER HEAT TREATMENT method is spiral scan pattern, and laser power is 1.5kW, and laser defocus distance is 30mm, light
Spot diameter is 40mm, and sweep speed is 40mm/s, and heating-up temperature is 400 DEG C, and target angle of inclination is 20 ° in scanning process, is obtained
To based on surface rapid thermal treatment high-purity compact magnesium oxide target.
Embodiment 5：
(1) with magnesium oxide powder as raw material, planetary ball mill is carried out to raw material, ball-milling medium is zirconia ball, during ball is differential
Ball：Bead is 2:1, rotational speed of ball-mill is 250r/min, and Ball-milling Time is 24h, and ratio of grinding media to material is 2.5:1, the powder after grinding is carried out
200 mesh sieves point, the purity of wherein magnesium oxide powder is not less than 99.99%, and impurity element total content is below 100ppm, average grain
Footpath is 150nm.
(2) powder after sieve is carried out into cold isostatic compaction, pressure is 200MPa, and the dwell time is 15min, obtains magnesia
Pressed compact, the wherein relative density of magnesia pressed compact are 61%, and relative density deviation is less than 2%.
(3) magnesia pressed compact is carried out into vacuum-sintering, room temperature is heated to 900 DEG C, is incubated 6h, and 5 are no more than with the rate of heat addition
DEG C/speed of min starts to vacuumize after being warmed up to 1000 DEG C, the sintering vacuum in 10min is 0.5Pa, then heating
Speed of the speed no more than 2 DEG C/min is warmed up to 1550 DEG C of sintering temperature from 1000 DEG C, is incubated 8h, after vacuum-sintering terminates, root
Surface accurate machining is carried out according to required target size obtain magnesium oxide target, wherein the average crystal grain chi of magnesium oxide target
Very little to be less than 7 μm, dimensional discrepancy is less than 3.0 μm, and surface roughness Ra is less than 0.4 μm.
(4) magnesium oxide target is carried out into surface grinding, then first removes piece surface greasy dirt with soap lye, then be with volume ratio
1:1:The mixed solution acid reagent of the sulfuric acid, 12wt% nitric acid and 14% hydrofluoric acid of 1 26wt% carries out Chemical cleaning, most
Grease is removed with acetone afterwards, finally surface rapid thermal treatment, scanning beam is carried out with scanning beam method under vacuum
The scan mode of method is overlap joint shuttle-scanning mode, and beam spot power density is 2.5kW/cm2, sweep speed is 30mm/s,
The speed of heating is 200 DEG C/s, and heating-up temperature is 350 DEG C, is obtained based on surface rapid thermal treatment high-purity compact magnesium oxide target.
Embodiment 6：
(1) with magnesium oxide powder as raw material, planetary ball mill is carried out to raw material, ball-milling medium is zirconia ball, during ball is differential
Ball：Bead is 3:1, rotational speed of ball-mill is 200r/min, and Ball-milling Time is 20h, and ratio of grinding media to material is 2.5:1, the powder after grinding is carried out
200 mesh sieves point, the purity of wherein magnesium oxide powder is not less than 99.99%, and impurity element total content is below 100ppm, average grain
Footpath is 150nm.
(2) powder after sieve is carried out into cold isostatic compaction, pressure is 200MPa, and the dwell time is 10min, obtains magnesia
Pressed compact, the wherein relative density of magnesia pressed compact are 59.6%, and relative density deviation is less than 2%.
(3) magnesia pressed compact is carried out into vacuum-sintering, room temperature is heated to 600 DEG C, is incubated 5h, and 5 are no more than with the rate of heat addition
DEG C/speed of min starts to vacuumize after being warmed up to 1000 DEG C, the sintering vacuum in 10min is 0.3Pa, then heating
Speed of the speed no more than 2 DEG C/min is warmed up to 1500 DEG C of sintering temperature from 1000 DEG C, is incubated 10h, after vacuum-sintering terminates, root
Surface accurate machining is carried out according to required target size obtain magnesium oxide target, wherein the average crystal grain chi of magnesium oxide target
Very little to be less than 7 μm, dimensional discrepancy is less than 3.0 μm, and surface roughness Ra is less than 0.4 μm.
(4) magnesium oxide target is carried out into surface grinding, then first removes piece surface greasy dirt with soap lye, then be with volume ratio
1:1:The mixed solution acid reagent of the sulfuric acid, 13wt% nitric acid and 12% hydrofluoric acid of 1 26wt% carries out Chemical cleaning, most
Grease is removed with acetone afterwards, finally surface rapid thermal treatment, non-phase is carried out with non-coherent broad band frequency Light Source Method under vacuum
The scan mode of dry broadband frequency Light Source Method is overall radiation mode, and non-coherent broad band frequency light source is graphite heater, the speed of heating
It is 80 DEG C/s to spend, and heating-up temperature is 400 DEG C, and soaking time is 8min, is obtained based on surface rapid thermal treatment high-purity compact oxidation
Magnesium target.
Comparative example：
(1) with magnesium oxide powder as raw material, carry out cold unidirectional compressing, pressure is 200MPa, and the dwell time is 8min,
Obtain magnesia pressed compact.
(2) magnesia pressed compact is carried out into vacuum-sintering, under air atmosphere, room temperature is heated to 500 DEG C, is incubated 4h, according to
Required target size carries out surface accurate machining and obtains high-purity compact magnesium oxide target.
Method of testing：The phase of magnesium oxide target prepared by embodiment 1-6 and comparative example is determined according to " cross " method
To density, after testing, the purity of magnesium oxide target prepared by embodiment 1-6 and comparative example, consistency, average grain size,
The result of dimensional discrepancy and Ra is as follows：
| Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 | Embodiment 5 | Embodiment 6 | Comparative example | |
| Purity (%) | 99.99 | 99.99 | 99.99 | 99.99 | 99.99 | 99.99 | 99.99 |
| Consistency (%) | 98.36 | 99.23 | 99.12 | 98.46 | 99.03 | 99.20 | 96.78 |
| Average grain size (μm) | 3.91 | 5.29 | 4.32 | 5.06 | 3.98 | 4.59 | 17.75 |
| Dimensional discrepancy (μm) | 1.21 | 2.38 | 1.89 | 2.03 | 2.13 | 1.67 | 5.12 |
| Ra(μm) | 0.254 | 0.297 | 0.286 | 0.267 | 0.271 | 0.281 | 0.523 |
As seen from the above table, the purity based on surface rapid thermal treatment high-purity compact magnesium oxide target and cause that prepared by the present invention
Density is high, and crystallite dimension is small, and surface smoothness is good, and surface is consistent with institutional framework with inside, it is possible to decrease the thickness on surface
Layer.
The above-described embodiments merely illustrate the principles and effects of the present invention, not for the limitation present invention.It is any ripe
The personage for knowing this technology all can carry out modifications and changes under without prejudice to spirit and scope of the invention to above-described embodiment.Cause
This, those of ordinary skill in the art is complete with institute under technological thought without departing from disclosed spirit such as
Into all equivalent modifications or change, should be covered by claim of the invention.
Claims (10)
1. a kind of preparation method based on surface rapid thermal treatment high-purity compact magnesium oxide target, it is characterised in that including following
Step：
(1) with magnesium oxide powder as raw material, planetary ball mill is carried out to raw material, rotational speed of ball-mill is 150-300r/min, Ball-milling Time
It is 8-32h, ratio of grinding media to material is 1.5-3:1, the powder after grinding carries out 200 mesh sieves point；
(2) powder after sieve in step (1) is carried out into cold isostatic compaction, pressure is 150-350MPa, and the dwell time is 5-
20min, obtains magnesia pressed compact；
(3) magnesia pressed compact in step (2) is carried out into vacuum-sintering, sintering temperature is 1400-1550 DEG C, and soaking time is 2-
10h, vacuum is 0.1-1.0Pa, after vacuum-sintering terminates, carries out surface accurate according to required target size and machines to target
Surface roughness≤0.8 μm, obtains magnesium oxide target；
(4) step (3) magnesium oxide target is carried out into surface grinding, is then cleaned, continuous wave is finally used under vacuum
LASER HEAT TREATMENT method, scanning beam method or non-coherent broad band frequency Light Source Method carry out surface rapid thermal treatment, obtain based on surface
Rapid thermal treatment high-purity compact magnesium oxide target.
2. a kind of preparation method based on surface rapid thermal treatment high-purity compact magnesium oxide target according to claim 1,
It is characterized in that：In the step (1), the purity of magnesium oxide powder is not less than 99.99%, and impurity element total content is 100ppm
Hereinafter, average grain diameter is 100-300nm.
3. a kind of preparation method based on surface rapid thermal treatment high-purity compact magnesium oxide target according to claim 1,
It is characterized in that：In the step (1), ball-milling medium is zirconia ball, the differential middle ball of ball：Bead is 1-3:1.
4. a kind of preparation method based on surface rapid thermal treatment high-purity compact magnesium oxide target according to claim 1,
It is characterized in that：In the step (2), the relative density of magnesia pressed compact is 58-62%, and relative density deviation is less than 2%.
5. a kind of preparation method based on surface rapid thermal treatment high-purity compact magnesium oxide target according to claim 1,
Characterized in that, in the step (3), the temperature-rise period of vacuum-sintering is：Room temperature is heated to 500-1000 DEG C, is incubated 4-10h,
Speed with the rate of heat addition no more than 5 DEG C/min is warmed up to after 1000 DEG C and starts to vacuumize, and the sintering vacuum in 10min is
0.1-1.0Pa, the speed for being then no more than 2 DEG C/min with the rate of heat addition is warmed up to 1400-1550 DEG C of sintering temperature from 1000 DEG C,
Insulation 2-10h.
6. a kind of preparation method based on surface rapid thermal treatment high-purity compact magnesium oxide target according to claim 1,
It is characterized in that：In the step (3), the average grain size of magnesium oxide target is less than 7 μm, and dimensional discrepancy is less than 3.0 μm,
Surface roughness Ra is less than 0.4 μm.
7. a kind of preparation method based on surface rapid thermal treatment high-purity compact magnesium oxide target according to claim 1,
Characterized in that, in the step (4), cleaning method is：Piece surface greasy dirt first is removed with soap lye, then is 1 with volume ratio:1:
The mixed solution acid reagent of the hydrofluoric acid of the sulfuric acid, 12-14wt% nitric acid and 12-14% of 1 24-26wt% carries out chemical clear
Wash, finally remove grease with acetone.
8. a kind of preparation method based on surface rapid thermal treatment high-purity compact magnesium oxide target according to claim 1,
It is characterized in that：In the step (4), the scan mode of continuous wave laser heat treating process is overlap joint shuttle-scanning mode or spiral
Scan mode, laser power is 1-3kW, and laser defocus distance is 20-50mm, and spot diameter is 10-50mm, and sweep speed is 1-
50mm/s, heating-up temperature is 350-450 DEG C, and target angle of inclination is 10 ° -30 ° in scanning process.
9. a kind of preparation method based on surface rapid thermal treatment high-purity compact magnesium oxide target according to claim 1,
It is characterized in that：In the step (4), the scan mode of scanning beam method is overlap joint shuttle-scanning mode or helical scanning side
Formula, beam spot power density is 1-3kW/cm2, sweep speed is 1-50mm/s, and the speed of heating is 100-200 DEG C/s, plus
Hot temperature is 350-450 DEG C.
10. a kind of preparation method based on surface rapid thermal treatment high-purity compact magnesium oxide target according to claim 1,
It is characterized in that：In the step (4), the scan mode of non-coherent broad band frequency Light Source Method is overall radiation mode, incoherent width
Band frequency light source is halogen light lamp, arc lamp, graphite heater or infrared equipment, and the speed of heating is 50-100 DEG C/s, heating-up temperature
It it is 350-450 DEG C, soaking time is 1-10min.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116874284A (en) * | 2023-07-13 | 2023-10-13 | 宁波江丰电子材料股份有限公司 | Preparation method of magnesium oxide target |
| CN116903349A (en) * | 2023-07-13 | 2023-10-20 | 宁波江丰电子材料股份有限公司 | Preparation method of large-size magnesium oxide target |
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2017
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116874284A (en) * | 2023-07-13 | 2023-10-13 | 宁波江丰电子材料股份有限公司 | Preparation method of magnesium oxide target |
| CN116903349A (en) * | 2023-07-13 | 2023-10-20 | 宁波江丰电子材料股份有限公司 | Preparation method of large-size magnesium oxide target |
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