CN109881243A - A kind of grinding technics of ultrahigh vacuum cavity - Google Patents
A kind of grinding technics of ultrahigh vacuum cavity Download PDFInfo
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- CN109881243A CN109881243A CN201910211324.2A CN201910211324A CN109881243A CN 109881243 A CN109881243 A CN 109881243A CN 201910211324 A CN201910211324 A CN 201910211324A CN 109881243 A CN109881243 A CN 109881243A
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- vacuum cavity
- ultrahigh vacuum
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- sealing surface
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- 238000000227 grinding Methods 0.000 title claims abstract description 24
- 238000005868 electrolysis reaction Methods 0.000 claims abstract description 51
- 238000007789 sealing Methods 0.000 claims abstract description 41
- 238000000034 method Methods 0.000 claims abstract description 31
- 238000001035 drying Methods 0.000 claims abstract description 27
- 238000004140 cleaning Methods 0.000 claims abstract description 26
- 238000006386 neutralization reaction Methods 0.000 claims abstract description 7
- 238000005498 polishing Methods 0.000 claims abstract description 5
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 60
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 58
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 56
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 30
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 29
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 28
- 238000007517 polishing process Methods 0.000 claims description 23
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 15
- 229910017604 nitric acid Inorganic materials 0.000 claims description 15
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 13
- 239000007788 liquid Substances 0.000 claims description 12
- 238000005491 wire drawing Methods 0.000 claims description 12
- 239000008399 tap water Substances 0.000 claims description 9
- 235000020679 tap water Nutrition 0.000 claims description 9
- 239000000243 solution Substances 0.000 claims description 8
- 239000007864 aqueous solution Substances 0.000 claims description 4
- 239000003599 detergent Substances 0.000 claims description 4
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 3
- 230000005611 electricity Effects 0.000 claims description 3
- 229910052710 silicon Inorganic materials 0.000 claims description 3
- 239000010703 silicon Substances 0.000 claims description 3
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims description 2
- 238000011017 operating method Methods 0.000 claims description 2
- 239000011734 sodium Substances 0.000 claims description 2
- 229910052708 sodium Inorganic materials 0.000 claims description 2
- 238000007602 hot air drying Methods 0.000 claims 1
- 229910052760 oxygen Inorganic materials 0.000 claims 1
- 239000001301 oxygen Substances 0.000 claims 1
- 230000000694 effects Effects 0.000 abstract description 9
- 238000012545 processing Methods 0.000 abstract description 5
- 239000012535 impurity Substances 0.000 abstract description 4
- 230000000052 comparative effect Effects 0.000 description 11
- 239000003792 electrolyte Substances 0.000 description 6
- 230000003749 cleanliness Effects 0.000 description 5
- 239000001307 helium Substances 0.000 description 5
- 229910052734 helium Inorganic materials 0.000 description 5
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 5
- 238000005259 measurement Methods 0.000 description 4
- 230000002378 acidificating effect Effects 0.000 description 3
- 239000004065 semiconductor Substances 0.000 description 3
- 238000005406 washing Methods 0.000 description 3
- 238000007605 air drying Methods 0.000 description 2
- 239000000428 dust Substances 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000005457 optimization Methods 0.000 description 2
- 239000002893 slag Substances 0.000 description 2
- 229910001220 stainless steel Inorganic materials 0.000 description 2
- 239000010935 stainless steel Substances 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000003796 beauty Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 230000003746 surface roughness Effects 0.000 description 1
- 238000004381 surface treatment Methods 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
Abstract
The invention discloses a kind of grinding technics of ultrahigh vacuum cavity, including prerinse, once electrolytic polishing, re-electrolysis polishing, secondary high-pressure cleaning, neutralisation treatment and three times high-pressure wash, in order to further increase the surface aesthetic effects of ultrahigh vacuum cavity, it further include the subsequent fine gtinding process to cavity sealing surface, the cleaning of four sub-high pressures and drying, ultrahigh vacuum cavity structural plane roughness after processing can reach the range of Ra 0.8~1.5, effectively reduce external waviness, and texture direction is consistent with line weight, it is few that impurity discharges gas flow, improve the surface quality of ultrahigh vacuum cavity component, the leakproofness in ultrahigh vacuum cavity element structure face has been effectively ensured.
Description
Technical field
The present invention relates to vacuum cavity surface treatment technical fields, and in particular to a kind of grinding of ultrahigh vacuum cavity
Technique.
Background technique
In semiconductor system equipment, to meet particular pressure condition required for semiconductor fabrication process, which must
Good leakproofness must be met.Wherein, ultrahigh vacuum cavity is a critically important component in semiconductor system equipment, it close
Envelope property well whether to system whether meet required condition serve it is key.It is the roughness of ultrahigh vacuum cavity structural plane, clean
Cleanliness is the key index for influencing ultrahigh vacuum cavity sealing performance, and the surface grinding process of ultrahigh vacuum cavity and superelevation are true
The sealing performance of cavity body structural plane is directly related.
Control and optimization to ultrahigh vacuum cavity structural plane sealing performance seek to fill that ultrahigh vacuum cavity is true to superelevation
The strict demand of reciprocal of duty cycle, wherein carrying out the optimization of grinding technics, to ultrahigh vacuum cavity structural plane to reduce ultrahigh vacuum cavity
The residual of surface impurity is the technical way for realizing ultrahigh vacuum cavity structural plane sealing performance, because in high vacuum ring
Under border, impurity and dirt can gasify as gas molecule, thus can a degree of vacuum degree for reducing vacuum cavity, so superelevation
The finish of vacuum cavity structural plane is higher, and the vacuum degree of ultrahigh vacuum cavity is better.
Summary of the invention
It is an object of the present invention to overcome defect existing in the prior art, a kind of grinding of ultrahigh vacuum cavity is provided
Technique, the roughness of ultrahigh vacuum cavity can reach the range of Ra0.8~1.5 after processing, effectively reduce cavity sealing surface
External waviness, and texture direction is consistent with line weight, and it is few that impurity discharges gas flow, improves ultrahigh vacuum cavity component
Surface quality, the leakproofness in ultrahigh vacuum cavity element structure face has been effectively ensured.
To achieve the above object, the technical scheme is to design a kind of grinding technics of ultrahigh vacuum cavity, superelevation
Material used in vacuum cavity is SUS304 stainless steel, including following operating procedure:
S1: prerinse is first cleaned the sealing surface of vacuum cavity using water-soluble alkaline detergent, is then used
The tap water of certain pressure carries out a high-pressure wash to the sealing surface of vacuum cavity, and dry；
S2: once electrolytic polishes, using the mixed liquor of sulfuric acid and phosphoric acid as once electrolytic in once electrolytic polishing process
Liquid, electrolysis temperature are 50~80 DEG C, and electrolysis time is 0.5~2min, and wherein the density of sulfuric acid is the density of 1.80g/mL, phosphoric acid
For 1.84g/mL, the volume ratio of sulfuric acid and phosphoric acid is 1: 2~2.5；
S3: re-electrolysis polishes, and the mixed liquor in re-electrolysis polishing process using nitric acid, sulfuric acid and phosphoric acid is as secondary
Electrolyte, electrolysis temperature be 60~90 DEG C, electrolysis time be 1~5min, wherein the density of nitric acid be 1.50g/mL, sulfuric acid it is close
Degree is 1.80g/mL, the density of phosphoric acid is 1.84g/mL, and the volume ratio of nitric acid, sulfuric acid and phosphoric acid is 0.8~1.0: 1: 2~2.5；
S4: it is clear to carry out secondary high-pressure to the sealing surface of vacuum cavity using the tap water of certain pressure for secondary high-pressure cleaning
It washes；
S5: neutralisation treatment neutralizes the sealing surface of vacuum cavity using the aqueous sodium carbonate of certain mass score
Processing；
S6: high-pressure wash and drying three times carry out the sealing surface of vacuum cavity using the pure water of certain pressure high three times
Pressure cleaning, and it is dry.
Grinding technics of the present invention is first cleaned ultrahigh vacuum cavity structural plane surface using alkaline cleaner, effectively
The oil-dirt for eliminating housing surface ensure that the working efficiency of subsequent once electrolytic polishing process and the use longevity of electrolyte
Life；Once electrolytic polishing process tentatively polishes ultrahigh vacuum cavity structural plane, eliminates ultrahigh vacuum cavity structural plane
Spatter dregs, slag inclusion, surface film oxide, re-electrolysis polishing process further throws ultrahigh vacuum cavity structural plane
Light effectively reduces the external waviness of vacuum cavity structural plane, while ensure that the finish of ultrahigh vacuum cavity structural plane, mentions
The high leakproofness of ultrahigh vacuum cavity structural plane；Neutralisation treatment operation effectively eliminate electrobrightening process twice remain to it is super
Corrosiveness of the electrolyte in high vacuum cavity body structure face to ultrahigh vacuum cavity structural plane；High-pressure wash uses pure water three times,
The remaining sodium carbonate liquor of ultrahigh vacuum cavity structural plane effectively is washed, ensure that the cleaning of ultrahigh vacuum cavity structural plane
Degree；Drying process ensure that the drying property of ultrahigh vacuum cavity finished product.
In order to effectively remove the dust and greasy dirt of ultrahigh vacuum cavity structural plane, preferred technical solution is the step
Water-soluble alkaline detergent in S1 is the mixed aqueous solution of sodium carbonate and sodium hydroxide, and wherein the mass percent of sodium carbonate is
2~5%, the mass percent of sodium hydroxide is 1~2%.
In order to guarantee the work limitation of once electrolytic polishing process and re-electrolysis polishing process, further preferred skill
Art scheme in addition, in the step S2 in once electrolytic polishing and S3 electrolysis unit used in re-electrolysis polishing process it is straight
Galvanic electricity source is provided by silicon controlled rectifier (SCR), and wherein DC voltage is 15 ± 5V, and electric current is 30000~35000A.
In order to effectively neutralize the acidic electrolysis bath that electrobrightening process twice remains to ultrahigh vacuum cavity structural plane, into one
Preferred technical solution is walked in addition, the mass percent of sodium carbonate is 20~30% in aqueous sodium carbonate in the step S5.
Wherein, aqueous sodium carbonate can not only effectively neutralize acidic electrolysis bath, while aqueous sodium carbonate is also convenient for washing clear, is convenient for
The progress of subsequent cleaning.
In order to guarantee the aesthetic effect of ultrahigh vacuum cavity finished product, further preferred technical solution is in addition, in the step
It further include that the fine gtinding process of cavity sealing surface, four sub-high pressures are cleaned and dried, described four times after the drying process of rapid S6
High-pressure wash cleans the sealing surface of vacuum cavity using the pure water of certain pressure.Wherein, the cleaning of four sub-high pressures and drying
It ensure that the cleanliness and drying property of finished product.
In order to further ensure the aesthetic effect of ultrahigh vacuum cavity finished product, further preferred technical solution is in addition, institute
Stating fine gtinding process is wire drawing process, and the direction of texture is consistent with thickness on vacuum cavity sealing surface after wire drawing process.It draws
Silk treated ultrahigh vacuum cavity finished product has beautiful grain effect, improves the aesthetic effect of product.
In order to guarantee the cleanliness of ultrahigh vacuum cavity in each step operational sequence, and cleaning standard is carried out for the next step
It is standby, preferred technical solution in addition, a high-pressure wash, secondary high-pressure cleaning, high-pressure wash and four sub-high pressures are clear three times
Washing middle water body pressure is 150~170Bar.
In order to guarantee the drying property of ultrahigh vacuum cavity finished surface, further preferred technical solution is in addition, described
Drying mode is heated-air drying, and drying temperature is 100~150 DEG C.
The advantages and beneficial effects of the present invention are:
1, grinding technics of the present invention is first cleaned ultrahigh vacuum cavity structural plane surface using alkaline cleaner, is had
Effect eliminates the oil-dirt of housing surface, ensure that the use of the working efficiency and electrolyte of subsequent once electrolytic polishing process
Service life；Once electrolytic polishing process tentatively polishes ultrahigh vacuum cavity structural plane, eliminates ultrahigh vacuum cavity structure
Spatter dregs, slag inclusion, the surface film oxide in face, re-electrolysis polishing process further throw ultrahigh vacuum cavity structural plane
Light effectively reduces the external waviness of vacuum cavity structural plane, while ensure that the finish of ultrahigh vacuum cavity structural plane, mentions
The high leakproofness of ultrahigh vacuum cavity structural plane；Neutralisation treatment operation effectively eliminate electrobrightening process twice remain to it is super
Corrosiveness of the electrolyte in high vacuum cavity body structure face to ultrahigh vacuum cavity structural plane；High-pressure wash uses pure water three times,
The remaining sodium carbonate liquor of ultrahigh vacuum cavity structural plane effectively is washed, ensure that the cleaning of ultrahigh vacuum cavity structural plane
Degree；Drying process ensure that the drying property of ultrahigh vacuum cavity finished product.
2, the water-soluble alkaline detergent in the step S1 is the mixed aqueous solution of sodium carbonate and sodium hydroxide, wherein carbon
The mass percent of sour sodium is 2~5%, the mass percent of sodium hydroxide is 1~2%, has effectively removed ultrahigh vacuum cavity
The dust and greasy dirt of structural plane ensure that the working efficiency of the electrobrightening process of next step.
3, in the step S2 in once electrolytic polishing and S3 electrolysis unit used in re-electrolysis polishing process it is straight
Galvanic electricity source is provided by silicon controlled rectifier (SCR), and wherein DC voltage is 15 ± 5V, and electric current is 30000~35000A, is guaranteed
The work limitation of once electrolytic polishing process and re-electrolysis polishing process.
4, the mass percent of sodium carbonate is 20~30% in aqueous sodium carbonate in the step S5.Aqueous sodium carbonate
Can not only effectively neutralize acidic electrolysis bath, at the same aqueous sodium carbonate be also convenient for washing it is clear, convenient for subsequent cleaning into
Row.
It 5, further include clear to the fine gtinding process of cavity sealing surface, four sub-high pressures after the drying process of the step S6
It washes and dries, the four sub-high pressures cleaning cleans the sealing surface of vacuum cavity using the pure water of certain pressure.Guarantee super
The aesthetic effect of high vacuum cavity finished product, the cleaning of four sub-high pressures and the dry cleanliness and drying property that ensure that finished product.
6, the fine gtinding process is wire drawing process, after wire drawing process on vacuum cavity sealing surface texture direction and line
Thickness is consistent.Ultrahigh vacuum cavity finished product after wire drawing process has beautiful grain effect, improves the beauty of product
Effect.
7, a high-pressure wash, secondary high-pressure cleaning, three times high-pressure wash and four sub-high pressures cleaning in water body pressure
It is 150~170Bar, guarantees the cleanliness of ultrahigh vacuum cavity in each step operational sequence, and carry out clearly for the next step
Clean preparation.The drying mode is heated-air drying, and drying temperature is 100~150 DEG C.It ensure that ultrahigh vacuum cavity finished surface
Drying property.
Detailed description of the invention
Fig. 1 is embodiment 1 to be shown using the texture of grinding technics of the present invention treated ultrahigh vacuum cavity seal groove inner wall
It is intended to.
In figure: 1, seal groove；2, surface texture.
Specific embodiment
With reference to the accompanying drawings and examples, further description of the specific embodiments of the present invention.Following embodiment is only
For clearly illustrating technical solution of the present invention, and not intended to limit the protection scope of the present invention.
Embodiment 1
Grinding technics of the invention is used to handle material for the ultrahigh vacuum cavity of SUS304 stainless steel, wherein
S1: prerinse is wiped using the sealing surface of sodium carbonate and the mixed aqueous solution vacuum cavity of sodium hydroxide first
Wash, wherein the mass percent of sodium carbonate is 3%, the mass percent of sodium hydroxide is 1.5%, then use pressure for
The tap water of 160Bar carries out a high-pressure wash to the sealing surface of vacuum cavity, and dry；
S2: once electrolytic polishes, using the mixed liquor of sulfuric acid and phosphoric acid as once electrolytic in once electrolytic polishing process
Liquid, electrolysis temperature are 60 DEG C, electrolysis time 1min, and wherein the density of sulfuric acid is 1.80g/mL, the density of phosphoric acid is 1.84g/
The volume ratio of mL, sulfuric acid and phosphoric acid is 1: 2；
S3: re-electrolysis polishes, and the mixed liquor in re-electrolysis polishing process using nitric acid, sulfuric acid and phosphoric acid is as secondary
Electrolyte, electrolysis temperature are 70 DEG C, electrolysis time 3min, and wherein the density of nitric acid is 1.50g/mL, the density of sulfuric acid is
1.80g/mL, phosphoric acid density be 1.84g/mL, the volume ratio of nitric acid, sulfuric acid and phosphoric acid is 0.8: 1: 2；
S4: secondary high-pressure cleaning uses pressure to carry out secondary height for sealing surface of the tap water of 160Bar to vacuum cavity
Pressure cleaning；
S5: neutralisation treatment neutralizes the sealing surface of vacuum cavity using the aqueous sodium carbonate of mass fraction 25%
Processing；
S6: high-pressure wash and drying three times use pressure to carry out three for sealing surface of the pure water of 160Bar to vacuum cavity
Sub-high pressure cleaning, and it is dry.
It further include that the fine gtinding process of cavity sealing surface, four sub-high pressures are cleaned after the drying process of the step S6
And drying, the four sub-high pressures cleaning clean the sealing surface of vacuum cavity using the pure water of certain pressure.It is described fine
Grinding process is wire drawing process, and the direction of texture is consistent with thickness on vacuum cavity sealing surface after wire drawing process.At wire drawing
In science and engineering sequence, housing surface texture with cavity transverse direction, is observed by bright light torch in parallel in the direction of wire drawing.
As shown in Figure 1, line of the embodiment 1 using grinding technics of the present invention treated ultrahigh vacuum cavity seal groove inner wall
Schematic diagram is managed, the surface texture 2 for wherein having cavity horizontally-parallel after wire drawing process on seal groove 1.
Embodiment 2
Embodiment 2 the difference from embodiment 1 is that, the mass percent of sodium carbonate is 2%, sodium hydroxide in step S1
Mass percent is 1%, and pressure is used to carry out a high-pressure wash for sealing surface of the tap water of 150Bar to vacuum cavity；Step
The volume ratio of sulfuric acid and phosphoric acid is 1: 2.5 in once electrolytic liquid in rapid S2, and wherein electrolysis temperature is 80 DEG C, and electrolysis time is
0.5min；The volume ratio of nitric acid, sulfuric acid and phosphoric acid is 1: 1: 2.5 in re-electrolysis liquid in step S3, and wherein electrolysis temperature is 60
DEG C, electrolysis time 1min；In step S5 using the aqueous sodium carbonate of mass fraction 30% to the sealing surface of vacuum cavity into
Row neutralisation treatment.
Embodiment 3
Embodiment 3 the difference from embodiment 1 is that, the mass percent of sodium carbonate is 5%, sodium hydroxide in step S1
Mass percent is 2%, and pressure is used to carry out a high-pressure wash for sealing surface of the tap water of 170Bar to vacuum cavity；Step
The volume ratio of sulfuric acid and phosphoric acid is 1: 2.3 in once electrolytic liquid in rapid S2, and wherein electrolysis temperature is 50 DEG C, and electrolysis time is
1.5min；The volume ratio of nitric acid, sulfuric acid and phosphoric acid is 0.8: 1: 2.2 in re-electrolysis liquid in step S3, and wherein electrolysis temperature is
80 DEG C, electrolysis time 5min；Using the aqueous sodium carbonate of mass fraction 20% to the sealing surface of vacuum cavity in step S5
It is neutralized.
Embodiment 4
Embodiment 4 the difference from embodiment 1 is that, the mass percent of sodium carbonate is 4%, sodium hydroxide in step S1
Mass percent is 1%, and pressure is used to carry out a high-pressure wash for sealing surface of the tap water of 150Bar to vacuum cavity；Step
The volume ratio of sulfuric acid and phosphoric acid is 1: 2.4 in once electrolytic liquid in rapid S2, and wherein electrolysis temperature is 70 DEG C, and electrolysis time is
2min；The volume ratio of nitric acid, sulfuric acid and phosphoric acid is 0.9: 1: 2 in re-electrolysis liquid in step S3, and wherein electrolysis temperature is 90 DEG C,
Electrolysis time is 4min；Using the aqueous sodium carbonate of mass fraction 28% in the sealing surface progress of vacuum cavity in step S5
And processing.
Comparative example 1
Comparative example 1 the difference from embodiment 1 is that, do not include step S1.
Comparative example 2
Comparative example 2 is with the difference of embodiment 1, only includes once electrolytic polishing process, wherein once electrolytic polishing process
It is middle using the mixed liquor of sulfuric acid and phosphoric acid as once electrolytic liquid, electrolysis temperature is 60 DEG C, electrolysis time 4min, wherein sulfuric acid
Density be 1.80g/mL, the density of phosphoric acid is 1.84g/mL, the volume ratio of sulfuric acid and phosphoric acid is 1: 2.
Comparative example 3
Comparative example 3 is with the difference of embodiment 1, only includes once electrolytic polishing process, wherein once electrolytic polishing process
Using the mixed liquor of nitric acid, sulfuric acid and phosphoric acid as once electrolytic liquid, electrolysis temperature is 70 DEG C, electrolysis time 4min, wherein
The density of nitric acid is 1.50g/mL, the density of sulfuric acid is 1.80g/mL, the density of phosphoric acid is 1.84g/mL, nitric acid, sulfuric acid and phosphorus
The volume ratio of acid is 0.8: 1: 2.
Comparative example 4
Comparative example 4 is with the difference of embodiment 1, to the essence of cavity sealing surface after the drying process not comprising the step S6
Fine lapping process, the cleaning of four sub-high pressures and drying.
The measurement of relevant parameter is carried out to each embodiment and comparative example, test result is referring to table 1.
1~4 test result of 1 Examples 1 to 4 of table and comparative example
Wherein the measuring method of vacuum degree is as follows: to cavity continuous air extraction 24 hours, measuring the minimum of its pressure, works as pressure
When power changing value is no more than 5% in 0.5 hour, taking gage readings peak is vacuum of the limit pressure as cavity
Degree.The measurement of leak rate is referring to GB/T 32218-2015: vacuum technique vacuum system leak rate test method.Flatness and parallel
The measurement of degree is referring to GB/T 1184-1996 shaped position tolerance.The measurement of roughness is referring to GB/T 1031-1995 rough surface
Spend parameter and its numerical value.
For being lower than (10-7~10-8)Pa.m3.s-1The molecular leak of standard air leak rate, helium (molecular weight 4) flow through in this way
Leak hole faster than air (molecular weight 29), i.e., helium leak rate correspond to lesser air leak rate, according to equivalent standard air leak rate
=√ (4/29) helium leak rate=0.37 helium leak rate can be derived that air leak rate.Numerical value in table it is found that made of using this technique
Its vacuum degree of cavity can reach the state of ultrahigh vacuum (UHV).
The results showed that using grinding technics of the invention treated ultrahigh vacuum cavity, performance is able to satisfy
The requirement of GB/T 1184-1996 and GB/T 1031-1995, and the vacuum degree of Examples 1 to 4, helium leak rate, surface roughness,
The parameter of flatness and the depth of parallelism is superior to the relevant experimental data of comparative example 1~4, illustrates that grinding technics of the invention effectively changes
It has been apt to the sealing surface performance in ultrahigh vacuum cavity element structure face, has realized goal of the invention.
The above is only a preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art
For member, without departing from the technical principles of the invention, several improvements and modifications can also be made, these improvements and modifications
Also it should be regarded as protection scope of the present invention.
Claims (8)
1. a kind of grinding technics of ultrahigh vacuum cavity, which is characterized in that including following operating procedure:
S1: prerinse first cleans the sealing surface of vacuum cavity using water-soluble alkaline detergent, then using certain
The tap water of pressure carries out a high-pressure wash to the sealing surface of vacuum cavity, and dry；
S2: once electrolytic polishes, using the mixed liquor of sulfuric acid and phosphoric acid as once electrolytic liquid, electricity in once electrolytic polishing process
Solving temperature is 50~80 DEG C, and electrolysis time is 0.5~2min, and wherein the density of sulfuric acid is 1.80g/mL, the density of phosphoric acid is
The volume ratio of 1.84g/mL, sulfuric acid and phosphoric acid is 1: 2~2.5；
S3: re-electrolysis polishes, and the mixed liquor in re-electrolysis polishing process using nitric acid, sulfuric acid and phosphoric acid is as re-electrolysis
Liquid, electrolysis temperature are 60~90 DEG C, and electrolysis time is 1~5min, and wherein the density of nitric acid is 1.50g/mL, the density of sulfuric acid is
1.80g/mL, phosphoric acid density be 1.84g/mL, the volume ratio of nitric acid, sulfuric acid and phosphoric acid is 0.8~1.0: 1: 2~2.5；
S4: secondary high-pressure cleaning carries out secondary high-pressure cleaning to the sealing surface of vacuum cavity using the tap water of certain pressure；
S5: neutralisation treatment is neutralized the sealing surface of vacuum cavity using the aqueous sodium carbonate of certain mass score；
S6: it is clear to carry out three sub-high pressures to the sealing surface of vacuum cavity using the pure water of certain pressure for high-pressure wash and drying three times
It washes, and dry.
2. the grinding technics of ultrahigh vacuum cavity as described in claim 1, which is characterized in that the water solubility in the step S1
Alkaline cleaner is the mixed aqueous solution of sodium carbonate and sodium hydroxide, and wherein the mass percent of sodium carbonate is 2~5%, hydrogen-oxygen
The mass percent for changing sodium is 1~2%.
3. the grinding technics of ultrahigh vacuum cavity as claimed in claim 2, which is characterized in that once electrolytic in the step S2
Polishing and the DC power supply of electrolysis unit used in re-electrolysis polishing process in S3 are provided by silicon controlled rectifier (SCR),
Wherein DC voltage is 15 ± 5V, and electric current is 30000~35000A.
4. the grinding technics of ultrahigh vacuum cavity as claimed in claim 3, which is characterized in that sodium carbonate in the step S5
The mass percent of sodium carbonate is 20~30% in solution.
5. such as the grinding technics for the ultrahigh vacuum cavity that claim 4 is stated, which is characterized in that in the drying process of the step S6
It afterwards further include the fine gtinding process to cavity sealing surface, the cleaning of four sub-high pressures and drying, the four sub-high pressures cleaning uses one
The pure water of constant-pressure cleans the sealing surface of vacuum cavity.
6. such as the grinding technics for the ultrahigh vacuum cavity that claim 5 is stated, which is characterized in that the fine gtinding process is wire drawing
It handles, the direction of texture is consistent with thickness on vacuum cavity sealing surface after wire drawing process.
7. the grinding technics of ultrahigh vacuum cavity as claimed in claim 6, which is characterized in that high-pressure wash, two
Water body pressure is 150~170Bar in sub-high pressure cleaning, three times high-pressure wash and the cleaning of four sub-high pressures.
8. the grinding technics of ultrahigh vacuum cavity as claimed in claim 7, which is characterized in that the drying mode is hot air drying
Dry, drying temperature is 100~150 DEG C.
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| CN201910211324.2A CN109881243B (en) | 2019-03-20 | 2019-03-20 | Grinding process of ultrahigh vacuum cavity |
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|---|---|---|---|
| CN201910211324.2A CN109881243B (en) | 2019-03-20 | 2019-03-20 | Grinding process of ultrahigh vacuum cavity |
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| CN109881243A true CN109881243A (en) | 2019-06-14 |
| CN109881243B CN109881243B (en) | 2020-01-21 |
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| CN201910211324.2A Active CN109881243B (en) | 2019-03-20 | 2019-03-20 | Grinding process of ultrahigh vacuum cavity |
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| CN115161649A (en) * | 2022-05-07 | 2022-10-11 | 电子科技大学 | Surface treatment method for metal part of molecular beam epitaxy equipment |
| CN115476278A (en) * | 2022-09-14 | 2022-12-16 | 江阴慕达斯真空设备有限公司 | Vacuum chamber surface treatment processing technology of vacuum coating machine |
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| CN109881243B (en) | 2020-01-21 |
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