CN1334358A - Process for preparing concentrated liquid specially adapted for chemical spray coating of Ni and its application method - Google Patents

Process for preparing concentrated liquid specially adapted for chemical spray coating of Ni and its application method Download PDF

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CN1334358A
CN1334358A CN 01127717 CN01127717A CN1334358A CN 1334358 A CN1334358 A CN 1334358A CN 01127717 CN01127717 CN 01127717 CN 01127717 A CN01127717 A CN 01127717A CN 1334358 A CN1334358 A CN 1334358A
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metallization
plating
treatment
water
constituent
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李伟善
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South China Normal University
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South China Normal University
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Abstract

A special concentrated liquid for chemical spray plating of Ni is prepared from pre-treating agent-1, pre-treating agent-2, metallizing agents A,B and C, and detergent through proportional mixing. It is applied through diluting it with non-ionic water, loading in pressure tank, closing said tank and regulation valve, switching on air compressor, regulating flow and spraying it onto surface of workpiece. Its advantages are high stability, easy dilution, no damage to workpiece, easy treatment of used liquid, and no environmental pollution.

Description

The preparation and the using method thereof of chemical plating nickel concentrated liquid specially
The present invention is the preparation and the using method thereof of chemical plating nickel concentrated liquid specially, belongs to the chemical plating technology.
In the electronic industry, the making of various microelectronics precision dies, before being used to produce mould in enormous quantities from duplicating of primary templates such as photoresist material laser image, information storage striped, microelectronic circuits, original nonmetal template surface need carry out metalized.Metallized non-metallic material original mould obtains metal grandmother plate through electroforming, and then the pan of constantly regenerating belongs to motherboard and even working plate, can produce microelectronic product in enormous quantities with working plate, the metallization of non-metallic material mould is one of gordian technique on the microelectronic product production line.On the one hand, if the method for metallising operational condition is inappropriate, can damage expensive nonmetal template, cause great financial loss, nonmetal template is to make through complicated technology, will be as the photoresist material template through multiple working procedures such as meticulous drawing, complicated optical system photography, flushings, cost is very high; On the other hand, metallized print effect (fidelity of reproduction) is determining the quality of product to a great extent, little figure that processes is extremely trickle on the non-metal board, and metal can be immersed in trickle depths when requiring metallization, otherwise the metal form that duplicates out is with serious distortion; The method for metallising of non-metal material surface has multiple, can classify as dry method and wet method.Dry method is meant the method for finishing under the high vacuum, plates as vacuum; Wet method promptly is the method for carrying out electroless plating in solution, and is the most ripe with electroless plated (plating piece is immersed in plating in the plating bath) silver-colored method in the wet method method for metallising.But electroless plated silver has many shortcomings, and subject matter is that the plating bath consumption is big, when especially plating piece is bigger, secondly is that plating bath is very unstable because the oxidisability of silver salt is extremely strong; For solving the problem that electroless plated silver exists, chemical plating silver method occurred, but chemical plating silver method there is the danger of contaminate environment and destructible plating piece; Plating bath sprays easy contaminate environment in the aerosol mode, and the spray of aerosol high pressure is toward plating piece, the plating piece of easy damaged fragility.The metallization that chemical silvering (no matter being electroless plated or chemical plating) obtains is crystalline structure, and the metal layer of crystalline structure is difficult to be immersed in the depths of trickle striped, thereby fidelity of reproduction is low; Electroless plated nickel is had to unformed metal layer usually, the subject matter of electroless plated nickel is that the plating bath consumption is big, the service temperature of middle pyrochemistry immersion plating nickel is higher, usually more than 70 ℃, thermally sensitive plating piece is extremely unfavorable, cryochemistry immersion plating nickel then requires to use strong alkali solution, and alkali-sensitive plating piece such as photoresist material are extremely unfavorable.
Purpose of the present invention be exactly for overcome and when solving that various microelectronics precision dies are made in the existing electronic industry nonmetal template surface method for metallising have that cost height, contaminate environment, fidelity of reproduction are poor, the shortcoming and the problem of fragile plating piece etc., study the preparation and the using method thereof of the metallized chemical plating nickel of nonmetal template surface concentrated liquid specially when invention is a kind of to be used for the making of microelectronics precision die, concentrated solution have long-term stability, easily dilution, plating bath do not damage plating piece, plating bath with the back easily handle, free from environmental pollution, coating has high frequency high fidelity.
The present invention realizes by following technical proposals: when the inventive method comprises that being used for precision die makes, and the compound method and the using method thereof of the metallized chemical plating nickel of primary template non-metal material surface concentrated liquid specially; Chemical plating nickel concentrated liquid specially comprises: six kinds of pre-treatment-1, pre-treatment-2, metallization A, metallization B, metallization C and metallization clean-out systems, wherein: the mixing formula ratio of each constituent of pre-treatment-1 is: tin protochloride SnCl 215~25%, hydrogenchloride HCl 15~25%, sodium cetanesulfonate C 16H 33SO 3Na0.1~0.3%, water H 2O 49.7~69.9%, and sensibilized is played in the dilution back; The mixing formula ratio of each constituent of pre-treatment-2 is: Palladous chloride PdCl 20.05~0.15%, hydrogenchloride HCl 15~25%, sodium cetanesulfonate C 16H 33SO 3Na 0.1~0.3%, water H 2O 74.55~84.85%, and activation is played in the dilution back; The mixing formula ratio of each constituent of metallization A is: single nickel salt NiSO 415~25%, quadrol C 2H 4(NH 2) 25~15%, sodium cetanesulfonate C 16H 33SO 3Na 5~15%, water H 2O 45~75%, and the required nickel that metallizes is worked to provide in the dilution back; The mixing formula ratio of each constituent of metallization B is: boric acid H 3BO 3: 20~40%, water H 2O 60~80%, and shock absorption is played in the dilution back; The mixing formula ratio of each constituent of metallization C is: sodium borohydride NaBH 47~9%, sodium hydroxide NaOH 15~25%, water H 2O 66~77%, and the mixing formula ratio that each constituent of reductive agent effect is played in the dilution back is; The mixing formula ratio of each constituent of metallization clean-out system is; Nitric acid HNO 30.5~1.5%, water H 2O 88.5~99.5%, and the dilution back plays a part to take off except that bad coating.
The using method of chemical plating nickel concentrated liquid specially of the present invention is as follows: 1. pre-treatment-1 and pre-treatment-2 usefulness deionized waters are pressed 1: 10 dilution proportion, divide and contain in two plastics spray bottles; 2. metallize A and metallization B with the dilution proportion of deionized water, mix in the metallization A/B mixed solution storage bottle that is placed in the chemical plating nickel pressure-pot by 1: 5; 3. metallize C with the dilution proportion of deionized water, place the metallization C liquid storage bottle in the chemical plating nickel pressure-pot by 1: 100; 4. metallize clean-out system with the dilution proportion of deionized water, place the metallization scavenging solution storage bottle in the chemical plating nickel pressure-pot by 1: 10; 5. at first seal pressure-pot, close variable valve, connect air compressor, regulate pressure, plating piece is carried out pre-treatment with the pre-treatment-1 and pre-treatment-2 solution that dilute less than 2 normal atmosphere (2atm); 6. open variable valve, connect A/B and C-channel (scavenging solution pathway closure this moment), the dilution plating bath of A/B mixed solution and C liquid is extruded by the low pressure that air compressor provides, the flow of regulating two kinds of plating baths is identical, and flow is 30 ml/min, after variable valve mixes, spray fan-shaped liquid level from nozzle, to the plating piece plating, plating finishes and closes variable valve, and the plating part cleans back power supply casting and uses; 7. if find the chemical plating layer problem is arranged, open variable valve, connect flushing channel (this moment, A/B and C-channel were closed), scavenging solution sprays with fan-shaped liquid level from nozzle equally, spray is toward bad coating, and therefore bad coating stripped, and plating piece carries out spraying plating again as stated above after cleaning.
The present invention compared with prior art has following advantage and beneficial effect: the plating bath of (1) spraying plating nickel of the present invention is deposited with concentrated solution form branch, thus stable, can standing storage, but dilution easily; (2) during plating of the present invention as long as dilute various concentrated solutions in proportion respectively, operate very easy; Before plating bath arrived plating piece, each component is mixing thoroughly, and it is neutral that plating bath is when arriving plating piece, thereby can not cause damage to plating piece; (3) each component of plating bath is nontoxic, and the plating bath consumption is few, with after be easy to collect and handle, thereby non-environmental-pollution problem; (4) metallization coating is noncrystal weave construction, thereby has high advantages such as fidelity of reproduction; (5) the present invention can overcome fully and solve have in the nonmetal template surface metallization technology when various microelectronics precision dies are made in the existing electronic industry that cost height, complex process, contaminate environment, fidelity of reproduction are poor, the shortcoming and the problem of fragile plating piece etc.
Embodiments of the present invention are more or less freely, as long as carry out mixed preparing by the various recipe ratios of the described chemical plating nickel of top specification sheets concentrated liquid specially, and carry out plating by the step-by-step operation of the described using method step of top specification sheets, just can implement the present invention preferably.The contriver has a lot of successful embodiment through years of researches, test.Below only for 3 embodiment be shown in table 1: table 1:
Figure A0112771700061

Claims (2)

1, a kind of compound method of chemical plating nickel concentrated liquid specially, it is characterized in that: chemical plating nickel concentrated liquid specially comprises: six kinds of pre-treatment-1, pre-treatment-2, metallization A, metallization B, metallization C and metallization clean-out systems, wherein: the mixing formula ratio of each constituent of pre-treatment-1 is: tin protochloride SnCl 215~25%, hydrogenchloride HCl 15~25%, sodium cetanesulfonate C 16H 33SO 3Na 0.1~0.3%, water H 2O 49.7~69.9%; The mixing formula ratio of each constituent of pre-treatment-2 is: Palladous chloride PdCl 20.05~0.15%, hydrogenchloride HCl 15~25%, sodium cetanesulfonate Cl 6H 33SO 3Na 0.1~0.3%, water H 2O 74.55~84.85%; The mixing formula ratio of each constituent of metallization A is: single nickel salt NiSO 415~25%, quadrol C 2H 4(NH 2) 25~15%, sodium cetanesulfonate C 16H 33SO 3Na 5~15%, water H 2O 45~75%; The mixing formula ratio of each constituent of metallization B is: boric acid H 3BO 320~40%, water H 2O 60~80%; The mixing formula ratio of each constituent of metallization C is: sodium borohydride NaBH 47~9%, sodium hydroxide NaOH 15~25%, water H 2O 66~77%; The mixing formula ratio of each constituent of metallization clean-out system is; Nitric acid HNO 3: 0.5~1.5%, water H 2O 98.5~99.5%.
2, a kind of using method of the chemical plating nickel concentrated liquid specially by claim 1 preparation, it is 1. pre-treatment-1 and pre-treatment-2 usefulness deionized water by 1: 10 dilution proportion, divides and contains in two plastics spray bottles; 2. metallize A and metallization B with the dilution proportion of deionized water, mix in the metallization A/B mixed solution storage bottle that is placed in the chemical plating nickel pressure-pot by 1: 5; 3. metallize C with the dilution proportion of deionized water, place the metallization C liquid storage bottle in the chemical plating nickel pressure-pot by 1: 100; 4. metallize clean-out system with the dilution proportion of deionized water, place the metallization scavenging solution storage bottle in the chemical plating nickel pressure-pot by 1: 10; 5. at first seal pressure-pot, close variable valve, connect air compressor, regulate pressure, plating piece is carried out pre-treatment with the pre-treatment-1 and pre-treatment-2 solution that dilute less than 2 normal atmosphere; 6. open variable valve, connect A/B and C-channel, the dilution plating bath of A/B mixed solution and C liquid is extruded by the low pressure that air compressor provides, the flow of regulating two kinds of plating baths is identical, and flow is 30 ml/min, after variable valve mixes, spray fan-shaped liquid level from nozzle, to the plating piece plating, plating finishes and closes variable valve, and the plating part cleans back power supply casting and uses; 7. find that the chemical plating layer has problem, open variable valve and connect flushing channel that equally with fan-shaped liquid level ejection, spray is toward bad coating from nozzle for scavenging solution, therefore bad coating stripped, and plating piece carries out spraying plating again as stated above after cleaning.
CN 01127717 2001-08-09 2001-08-09 Process for preparing concentrated liquid specially adapted for chemical spray coating of Ni and its application method Pending CN1334358A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102909078A (en) * 2012-10-25 2013-02-06 南京大地冷冻食品有限公司 Non-metallic material chemical plating high-activity palladium catalyst concentrated solution and preparation method thereof
CN103485171A (en) * 2013-09-22 2014-01-01 武汉纺织大学 Non-target spray activation method for fabric chemical plating

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102909078A (en) * 2012-10-25 2013-02-06 南京大地冷冻食品有限公司 Non-metallic material chemical plating high-activity palladium catalyst concentrated solution and preparation method thereof
CN102909078B (en) * 2012-10-25 2014-09-24 南京大地冷冻食品有限公司 Non-metallic material chemical plating high-activity palladium catalyst concentrated solution and preparation method thereof
CN103485171A (en) * 2013-09-22 2014-01-01 武汉纺织大学 Non-target spray activation method for fabric chemical plating

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